In the Name of Allah most

Merciful most Gracious

Chemist
 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

Introduction

Have you ever sat down and had open discussion over coffee with chemist or chemical
technician about his or her work? Have you ever “shadowed” a chemist or a chemical
technician for a day as he or she went about the daily routine in laboratory? If you have done
these things, you were likely surprised at how foreign the language seemed or startled at
how unfamiliar surroundings were, despite what you perceived as your thorough academic
grounding in principles of chemistry. Is there any talk of quantum mechanical model of the
atom? No. Is there any activity relating to the molecular orbital theory of bonding? No.

Do you hear anything about safety in laboratory? Yes! In fact, if you visited a lab, you
had to go through some sort of safety check, such as reading basic safety guidelines, prior to
even entering facility. You probably also had to “sign in” and be issued personal protective
equipment, such as safety glasses and a lab coat. If you later followed a chemist into
production facility to take samples, you may have been issued a hard hat or perhaps a small
white disposable stretch-cap to cover your hair.

If you toured a lab facility, you probably toured a “wet lab,” a “quality control lab,” or
perhaps a “process development lab,” or maybe all of the above and wondered what these
terms meant. You probably saw a control chart and wondered what it was. You may have sat
in on a meeting to prepare for the upcoming quality assurance audit and wondered what an
audit actually was or what GLP, MSDS, and SOP meant. You may have encountered
a formal means of disposing of chemical waste and said, “Wow!” Or you may have noticed
an experiment or an instrument that wasn’t working properly and, subsequently, observed
chemists and technicians teaming together for troubleshooting.

Chemical laboratory requires a variety of skills and this course intends to address some
of the basic issues by providing introductions, explanations and examples to help laboratory
staff to develop analytical skills. Reference is made to best practices and industry standards.

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

Chemical Laboratory, historical and review

Chemistry is the science of matter, its properties, and changes. It is not just information.
It is also a process for finding out more about matter and its changes. Laboratory activities
are the primary means that chemists use to learn more about matter. The activities in the
Laboratory require that you form and test hypotheses, measure and record data and
observations, analyze those data, and draw conclusions based on those data and your
knowledge of chemistry. These processes are the same as those used by professional
chemists and all other scientists.

Where should the laboratory be located? How much space is required? Will a proposed
layout contribute to smooth traffic flow? What utilities are needed? What safety factors
should be built in? These are just some of the major questions planners must address. The
results of poor planning usually do not show up until a facility has been in operation for
some time. By then, correcting them is invariably expensive. Anyone who has worked in
a laboratory for even a short period has seen some of these problems.

There may be overcrowded workbenches, where permanent equipment and set-ups

leave little or no room for non-routine work, or inadequate wiring which requires the use of
cumbersome and hazardous extension cords on a permanent basis. Poor ventilation is
a common problem, causing both discomfort and hazards. Improperly chosen bench tops
may be stained by chemicals or damaged by heat. Many laboratories have awkward traffic
patterns, resulting in wasted time during performance of routine tasks.

Storage areas may be inadequate or poorly located. The list goes on and on. Many will
blame such problems on lack of funds when the laboratory was built. This may not be the
case. A well-planned and efficient laboratory does not have to cost more than a poorly
planned one. It is mostly a matter of putting the available money to work where it counts
most. It also presents cases where additional money spent at the outset has paid off in a safer
and more efficient operation for years to come.

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

Laboratory design considerations

A laboratory may come in any size or shape. It may be a room in an industrial plant,
a wing of a hospital, or a whole building on a college campus. All of these present similar
problems and decisions at the planning stage.

Who plans and builds a laboratory? In a small facility the whole job is often handled by
in-house talent. We seen many cases where such talent was capable of taking on the
challenge. We also seen numerous cases where professional assistance should have been
employed. This course will help the do-it-yourselfer decide when such assistance is needed.

The exact location of a laboratory within a building or a complex of buildings is often

the result of a grand compromise. Sometimes the laboratory planner is presented with
a location and must simply make the best of it. If the location is poor, he will then have to
use his best persuasive powers to bring about a change. What arguments are effective against
a poor location? If insufficient space is problem, a careful estimate of space requirements,
prepared as described, will help the planner prove his point. In other cases, the cost of
conversion can be presented as a forceful deterrent. A medical laboratory, for example, is
often located in a multi-purpose suite of a medical center. Such a suite may not be adaptable
for laboratory use without expensive modification.

Time has now come to convert the preceding data and ideas to a workable laboratory
layout. In all but the simplest cases this should be done with the assistance of a contractor,
designer, engineer, or other building professional. Many small laboratories are planned
strictly on a do-it-yourself basis in order to save money. Unless an experienced in-house
person happens to be available, the results are often poor and the savings questionable.

In other cases, whole job is turned over to an architectural or engineering on a turn-key

basis with little involvement by the laboratory operator. This sometimes results in a facility
that is not altogether suitable for its intended functions, in spite of a highly professional
design. Some designers tend to rely heavily on standard layouts which they have used
successfully in the past but which may not be suitable for a given installation.

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

Laying out the laboratory will be accomplished under one of three conditions. In the
first, and most desirable, the laboratory will be incorporated into a building still in the
planning stage. In this situation, there will be some leeway in organizing the shape of the
area, even though the location and overall space allowance may already have been
determined. Somewhat less desirable, but quite workable, is placing the laboratory in
a partitioned off section of an existing building. In either of these cases, the laboratory
operator, in close cooperation with the designer or architect, will have to spend much time
selecting the best room sizes and dimensions.

The greatest challenge comes in the third situation, in which one or more existing
rooms are simply designated by management as "laboratory" and must be utilized to their
best advantage. Whatever building limitations the planner finds himself working under, he
must make certain that there is indeed enough square footage available for the laboratory. If
not, this is the time to call for major changes.

If the space seems large enough based on preliminary estimates, planning for the best
utilization of this space may now proceed. Detail drawings will show if not only the size but
the shape of the room will suit the requirements of a laboratory.

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

Room Organization: Sketching on copies of the drawing may now start. If walls are to
be put up, a thickness of 6 inches may be assumed, unless special circumstances are present.
Preferable door width is 36 inches, but 30 inches may be acceptable under some local codes.
Installation of large equipment, could require larger (double) doors, generally five feet wide.
For safety reasons, a laboratory must have two exits. Using the space requirements
previously developed, tentative placement of specific pieces of equipment may now be
made. Planners should try to visualize the daily laboratory routine while doing this.
Anything that will save steps and minimize congestion should be incorporated.

Floors: Immediately clean up any spill, including water, and any broken glass. If spilled
material is hazardous follow procedures of safety. A broom and dust pan is available in the
chemicals lab. Do not store chemical or instruments on floors. Do not leave empty boxes or
packaging materials on the floor.

Work Bench Space: The first step in space planning should be to estimate how much
bench space "will be required. Benches must accommodate various pieces of permanently
installed equipment and still have room for both frequently performed and special one-time
tasks. Benches may be either installed against the wall or placed back to back in peninsulas
or islands. The exact configuration will be worked out later.

For now, what is important is the total number of running feet of bench space that will
be required. All bench-mounted equipment should be listed with its dimensions, which can
be taken from measurements or from catalog data. It should be noted which instruments may
have to be put at a certain minimum distance from other objects in order to avoid
interference or allow for servicing.

Work space should be allowed next to each instrument for samples, notebooks, etc.
This space may be considerable in case of an analytical instrument on which many samples
are to be tested at one time. Space sharing should be discouraged, with the required work
space next to an instrument reserved for that alone. Sinks and fume hoods should also be
included in list, with an allowance of at least 18 inches of free space on each side of a sink.

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 Chemical laboratory; Operations, Equipment,
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When all equipment has been listed, the total number of running feet needed can be
added up. How much more will be required? This will vary from one laboratory to another.
In an industrial laboratory where both routine testing and product development work are to
be performed, this figure can safely be multiplied by four for a realistic estimate. In some
laboratories used exclusively for specific types of work with no other types contemplated,
this figure may be lower. It should be kept in mind, however, that expanding an existing
laboratory is an extremely expensive undertaking. It is desirable, therefore, to have some
unused wall space and some free floor area when a new laboratory begins operation.

Free-standing equipment must also be considered. This includes refrigerators, safety

storage cabinets for chemicals, safety shower, desk space, computer terminal, or any other
equipment that is not bench mounted. File cabinets, are real space-robbers, must not be
forgotten. In one laboratory, much space was saved by placing two-drawer file cabinets
beneath the large table used for sorting samples.

Keep bench tops clear of waste paper, dirty glassware, sample bottles, gloves, lab coats,
stock chemicals, tools, etc. Return all items to proper storage immediately after use. Sponge
off any excess water on bench tops. Do not allow water to drip off bench tops to drawers or
cabinets below. Immediately clean up any minor spills of dry or liquid chemicals on bench
tops. If the spilled material is hazardous, follow the procedures of safety.

When working with corrosive chemicals on bench tops use absorbent sheets to protect
the bench top. Dispose of sheets or wash off clean sheets for reuse. Do not tape off sections
of bench top to reserve work space. If it is necessary to tape off bench tops, do not leave tape
on for long periods as tapes becomes difficult to remove.

Additional Space: Careful scrutiny of all measurements will soon show a laboratory
planner that much more space is required than was originally thought. Next comes the
competition for this space, at which time convincing evidence must be produced. One
laboratory manager proudly showed off his new facility, the product of such a battle. Yes, he
had been accused of taking up far more space than he really needed. He had done his

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 Chemical laboratory; Operations, Equipment,
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homework, however, and presented management with enough data to convince them.
Although his laboratory had much free floor space and a whole empty wall, he had looked
into future plans and knew what would be required before too long. He also had spare
circuits in the breaker box and plumbing which could readily be expanded.

Planning for Future: There was general rejoicing in a community college chemistry
department a few years ago when funds were granted for a long desired expensive analytical
instrument. Then someone realized there was really no good place to put it, so a make-shift
arrangement had to be made. Planners of this nearly new facility should considered such
equipment additions in their preliminary calculations, in anticipation of day when funds
might become available.

Storage Areas: When it comes to laboratory storage, it is safe to say that the space
required is at least twice what a planner would estimate. Samples, reagents, and spare
equipment will pile up at an alarming rate. To this should be added the fact that some items
will have to be stored under controlled conditions and that valuable iten1s will need to be
kept in locked storage. Flammables, even in moderate amounts, need special storage. Since
regulations vary from one area to another, this matter should be discussed with local file
department officials.

Laboratory storage cabinets and shelves are available in different widths and are
usually 12 inches deep. A depth of more than this is not recommended unless large, bulky
items are to be stored. Narrower shelves, six to nine inches deep, have been found more
practical for reagents and other small items. If shelves and cabinets are to be mounted on
Talls above work benches, possible interference with work performed there must be
considered. Three feet or more should be allowed for aisles.

Sample Receiving area: Analytical laboratories need an area where incoming samples
can be sorted and recorded. The size of this is hard to overestimate. In addition, some
laboratories need an area where samples can be prepared. A pesticide laboratory, for
instance, may want to set aside a complete room for such work, since it is often quite messy.

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

Laboratory Utility Requirements

A typical laboratory will require a variety of common utilities, such as water, gas, and
electric power. There must also be sewer connections and adequate provision for ventilation,
as well as means for heating and cooling the area.

In addition, there are often special laboratory needs, such as compressed air and
vacuum. At this point of the planning, we are mainly concerned with quantitative estimates
of such utilities and the ease, or lack thereof, with which they can be brought to the
laboratory area. These considerations have a profound effect on laboratory layout.

In laboratories that have been in operation for some time, a lack of needed utilities is a
major problem, particularly when new procedures are introduced. Estimates should be made
by the laboratory operator in close cooperation with building professionals and should take
future needs into consideration.

Hot and Cold Water: Most laboratories have relatively modest requirements for water,
but it must be available in the right places. Some planners find it useful to terminate rough
plumbing near a corner of a room, thereby making it easier to extend the finished plumbing
along two walls. Rough plumbing may be run below the floor, inside the walls, or in the
ceiling. Plans for this should be made in conjunction with the detailed room layout.

Determining the number of sinks needed and their approximate location at this point,
moreover, will be of great help to the designer. The laboratory operator should be able to
assist a professional estimator determine the water heater size from his knowledge of work
to be performed. It is often practical and economical to have one heater serve a fairly large
area, as long as the distance from heater to points of usage is not excessive.

A testing laboratory which was located in a long, narrow building, on the other hand,
found it more suitable to install two smaller heaters, one at each end of the building.
Insulating hot water lines is highly recommended. In hard water areas, a water softener will
increase the life of water heaters and plumbing fixtures.

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 Chemical laboratory; Operations, Equipment,
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Deionized Water: A still used to be a fixture in laboratories. Older chemists have

unpleasant memories of the occasional cleanouts that needed to be made. Today laboratories
have found that deionized water will serve most of their purposes just as well at a much
lower cost. Rental-type deionizers are available from several companies, who will install the
resin tanks and exchange them as needed. There is usually an installation charge, a fixed
monthly charge, and a separate charge each time a tank is changed. The service company
will make an estimate as to what size tank or tanks a laboratory needs.

The use of two tanks in series is highly recommended. When one gives out, the other
will take over until the service company arrives. This avoids annoying delays that are bound
to occur should a single tank stop operating at some crucial moment. The condition of a DI
water tank is indicated by a small neon light. When the light goes out, the tank is exhausted.
Since the power consumption of the light is very low, it can be plugged in to any available
circuit. DI water is not equivalent to distilled water in all ways. While the content of most
ionic species is very low, it does contain dissolved gases, such as air and carbon dioxide.

The latter caused problems in one laboratory when DI water was used for diluting
poorly buffered samples for pH measurements. Erratic results were also reported in another
case when DI water was used in connection with the determination of trace amounts of
boron. The manufacturer explained that when close to exhaustion, the resin used would no
longer be effective in holding back traces of this element.

Finally, DI water is anything but sterile. In fact, the resin beds seem to support bacterial
growth quite well. In other words, it does not replace distilled water for all applications, but
those who use it right will enjoy pure water at reasonable prices. DI water is handled in
plastic pipe, generally PVC. For rough plumbing, it is usually desirable to have the pipe
terminate close to the hot and cold water lines. Tanks should be located where servicing will
be convenient and where water spills minor during tank exchange will cause no problems.
One laboratory placed them in a small closet with a door leading to the outside of the
building, where the service truck could park directly in front of the door.

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 Chemical laboratory; Operations, Equipment,
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Distilled Water: There are times when DI water just will not do, as seen in the above
examples. Distilled water is then required. A laboratory may distill some of its DI water,
which will give the still a longer life. On a large college campus, steam was available from
the central heat generating plant, an ideal source of distilled water. Then there are cases
where ultra-pure water is required for special purposes. This is best produced from
previously purified water in all-glass apparatus under carefully controlled conditions.

Gas: For many years, gas was the primary source of heat in the laboratory. Today,
although electric heaters have become more common, gas still has some advantages
sometimes overlooked. It is a quick source of heat and very fast to regulate. A gas burner
can be pulled away in a fraction of a second should a distillation or a reflux operation get out
of hand. In case of a spill, a gas burner is quickly dismantled and cleaned, whereas an
electric heating element may have to be replaced.

Another advantage is the lower cost of the gas burners. Running gas lines into
a laboratory is not difficult once it has been determined where they are needed. It may
simplify plumbing installation to have rough plumbing for gas terminate close to the water
lines. When estimating total requirements for gas, it should be kept in mind that it may also
be needed for a water heater and a heating unit for the building.

Electric Power: In laboratories in operation for some time, there are often not enough
electrical outlets or enough circuits to handle the load. Retrofitting for more power is very
expensive. One laboratory received several bids for wiring their new facility. The accepted
one was much lower than the others because money was saved by installing the bare
minimum number of circuits and no spare circuit breakers.

Every piece of conduit was jammed full of wires. Within two years, more wiring was
needed for new equipment. This very costly expansion would not have been necessary if
allowance had been made for future work. From the list of laboratory operations previously
prepared, it will now be easy to single out the ones that require power.

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

The manuals for the equipment already on hand and catalog information on items yet to
be purchased can provide the power requirements. Compared to what was available some
years ago, modern laboratory equipment does not need much power. Exceptions are heating
devices and motors, which may be very power hungry. A list of the wattages involved
should be made, noting which equipment operates on 110 volts and which on 220.

Allowance should be made for future purchases of equipment. This information will
help the electrical engineer or contractor determine the number of circuits. Most modern
instruments will operate over a wide voltage range but they may, at the same time, be quite
sensitive to voltage variations during use. Such variations often throw calibrations off, as
they did in one laboratory where an AA spectrophotometer suddenly began to act up.

Investigation showed that someone had plugged a large hot plate into the same circuit
in another room. As the proportional switch in the plate went on and off, the circuit suffered
enough voltage variation to affect the instrument. High wattage equipment was from then
on kept off this circuit.

Compressed Air and Vacuum: Power requirements for compressors and vacuum pumps
must be considered when wiring plans are made. Both compressed air and vacuum are
frequently used in laboratories. Sometimes both can be piped to more than one laboratory
room from a central location. Air pressure sufficient for laboratory applications, but vacuum
may not always be, in which case a separate vacuum pump would be required.

Even a small compressor tends to be very noisy and for that reason should not be in the
laboratory proper. Rough plumbing will carry air to the laboratory area.

Since the moisture in compressed air causes rusting, use of rust-resistant pipe will
substantially lengthen the life of the air filters. Vacuum pumps, on other hand, are usually
not too noisy to be in laboratory, although the pump selected should be checked for noise
before such a decision is made.

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

Ventilation: A well-ventilated laboratory is still not as common as it ought to be. While

local building codes may not require it, any laboratory should have a well-designed forced
ventilation system. It not only promotes worker comfort but has a strong effect on safety.
Many designers of ventilation systems treat a laboratory like an office, calculating the
volume of the area and using standard formulas for planning the system. Under some
conditions this works very well and conserves much energy for both heating and cooling.

The typical ventilation system recirculates a major portion of the air, however, and in
many laboratories this is not acceptable. Even though work creating significant amounts
of hazardous or unpleasant fumes is performed in hoods, many fumes may still come from
the work bench. In addition, non-hazardous amounts of corrosive fumes will in time have
their effect on metals.

The ideal laboratory ventilation system is the once-through type, where all air is
exhausted to the outside after a one-way trip through the area. It is expensive because it
raises both heating and cooling requirements, but it will still payoff. In one laboratory with
such a system, small amounts of corrosive vapors, far from enough to be called hazardous,
would occasionally develop.

No proposal for a laboratory ventilation system should be requested without a thorough

study of the work to be performed. A once-through system may not always be required. The
manager of a research laboratory, working closely with a designer, discovered that 50%
recirculation would be permissible in their new building.

While this is even less than in offices and stores, it proved to be adequate for their type
of work. He would not recommend this ratio for other laboratories without a careful study.

Heating and Cooling: A good heating and air conditioning system provides more than
creature comfort for those working in a laboratory. Conditions of reasonably constant
temperature and humidity are important for the proper performance of many laboratory
operations. Conventional hot-air furnaces, similar to those found in homes, are often used in

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 Chemical laboratory; Operations, Equipment,
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laboratories. A university campus or an industrial plant may have steam available, which can
be conveniently put to use for heating.

Air conditioners are frequently combined with heaters. A convenient place must be
found for the compressor, generally outdoors. Heat pumps have been used a great deal in
recent years with satisfactory results.

In very dry climates, laboratories often install evaporative coolers because of their
reasonable cost of installation and operation. Their one drawback, sometimes serious, is that
the inside air tends to become uncomfortably humid.

Estimating the amount of heat, cooling, or air flow required is a job for a skilled
professional. Such an expert should also be called in when it seems desirable to extend
a system to areas other than those for which it was originally designed.

Finally, is it permissible to build a laboratory in the proposed location? Some regulation

could make the project impractical or even impossible. Generally there is little problem
getting permission on a college campus or in an industrial plant, although this must be
checked out with the proper authorities. The situation becomes quite different if a new
building is to be erected for laboratory use or if an existing building is to be converted.
Zoning regulations must be considered and an opinion from local planning authorities must
be obtained before further planning can take place.

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 Chemical laboratory; Operations, Equipment,
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Laboratory Operation

Laboratory Glassware and Plastic ware

Laboratory glassware and Plastic ware refers to a variety of equipment, traditionally

made of glass, used for scientific experiments and other work in science, especially in
chemistry and biology laboratories. Some of the equipment is now made of plastic for cost,
ruggedness, and convenience reasons, but glass is still used for some applications because it
is relatively inert, transparent, more heat-resistant than some plastics up to a point, and
relatively easy to customize.

Borosilicate glasses are often used because they are less subject to thermal stress and
are common for reagent bottles. For some applications quartz glass is used for its ability to
withstand high temperatures or its transparency in certain parts of the electromagnetic
spectrum. In other applications, especially some storage bottles, darkened brown or amber
(actinic) glass is used to keep out much of the UV and IR radiation so that the effect of light
on the contents is minimized. Special-purpose materials are also used; for example,
hydrofluoric acid is stored and used in polyethylene containers because it reacts with glass.
For pressurized reaction, heavy-wall glass is used for pressure reactor.

There are many different kinds of laboratory glassware items. Such glassware is used
for a wide variety of functions which include volumetric measuring, holding or storing
chemicals or samples, mixing or preparing solutions or other mixtures, containing lab
processes like chemical reactions, heating, cooling, distillation, separations including
chromatography, synthesis, growing biological organisms, spectrophotometry, and
containing a full or partial vacuum, and pressure, like pressure reactor. When in use,
laboratory glassware is often held in place with clamps made for that purpose, which are
likewise attached and held in place by stands or racks.

Most laboratory glassware is now mass-produced, but many large laboratories employ
a glass blower to construct specialized pieces. This construction forms a specialized field of
glassblowing requiring precise control of shape and dimension.

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In addition to repairing expensive or difficult-to-replace glassware, scientific

glassblowing commonly involves fusing together various glass parts—such as glass joints
and tubing, stopcocks, transition pieces, and/or other glassware or parts of them to form
items of glassware, such as vacuum manifolds, special reaction flasks, etc. Various types of
joints and stopcocks are available separately and come fused with a length of glass tubing,
which a glassblower may use to fuse to another piece of glassware.

Borosilicate glass, which makes up the majority of lab glass, may fracture if rapidly
heated or cooled through a 150 °C (302 °F) temperature gradient. This is particularly true of
large volume flasks, that can take hours to safely warm up. Gentle thermal cycling should be
used when working with volumes more than hundreds of mLs to two liters. Whenever
working with borosilicate glass, it is advisable to avoid sharp transitions between
temperatures when the heating and cooling elements have a high thermal inertia. Glassware
can be wrapped with tinfoil or insulated with wool to smooth out temperature gradients.

500 °C (932 °F) is the maximum service temperature for borosilicate glass as, at 510 °C
(950 °F), thermal strain begins to appear in the structures. Operation at this temperature
should be avoided and only intermittent. Bear in mind that glassware under vacuum will also
have around one atmosphere of pressure on its surface before heating and so will be more
likely to fracture as temperature transitions increase. Vacuum operation should be used if the
atmospheric temperatures required are above a few hundred degrees Celsius, as this often
has a dramatic effect on boiling points; significantly lowering them. Borosilicate anneals at
560 °C (1,040 °F), this removes built in strain in the glass. At 820 °C (1,510 °F), borosilicate
glass softens and is likely to deform. And at 1,215 °C (2,219 °F) it becomes workable.

Quartz glass is far more resilient to thermal shock and can be operated continuously at
1,000 °C. Thermal strain appears at 1,120 °C, annealing occurs at 1,215 °C, and it becomes
workable at 1,685 °C.

A thin layer of grease is usually applied to the ground-glass surfaces to be connected,

and the inner joint is inserted into the outer joint such that the ground-glass surfaces of each

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 Chemical laboratory; Operations, Equipment,
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are next to each other to make the connection. The use of grease helps to provide a good seal
and prevents the joint from seizing, allowing the parts to be disassembled easily. Using
greases specifically designed for vacuum is also a good idea, as these are often better at
sealing under vacuum, thicker and so less likely to flow out of the taper, become fluidic at
higher temperatures than Vaseline (a common substitute) and are more chemically inert than
other substitutes. Grease allows easily to see when a taper is leaking, as bubbles can usually
be seen flowing through the taper.

When contamination is a serious concern, Poly-tetra-fluoro-ethylene PTFE (Teflon)

sleeves and PTFE sealing rings can be used in between joints to fit them together instead of
grease. PTFE tape can also be used, but requires a little care when winding onto the joint
to ensure a good seal is produced. Keck clips and other clamping methods can be used to
hold glassware together.

Cleaning glassware and plastic ware: There are many different methods of cleaning
laboratory glassware. Most of the time, these methods are tried in this order:

- It is soaked in a detergent to remove grease and loosen most contamination.

- Glassware should be rinsed with tap water followed by deionized & distilled water and
placed in drying racks.

- Gross contamination and large particles are removed mechanically, by scrubbing with
a brush or scouring pad.

- Alternatively, the first two steps may be combined by sonicating the glassware in a hot
detergent solution.

- Solvents used to rinse glassware and remove last traces.

- Acetone is often used for a final rinse of sensitive or urgently needed glassware as the
solvent is miscible with water, and helps dilute and wash away remaining water.

- Glassware is often dried by suspending it upside down to drip dry on racks; these can
include a hot air fan to blow the internals dry. Another alternative is to place the
glassware under vacuum, lower the boiling points of the remaining volatiles.
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- If the glassware are still dirty, more drastic methods may be needed. This includes
soaking the piece in a saturated solution of sodium or potassium hydroxide in an
alcohol "base bath", followed by a dilute solution of hydrochloric acid "acid bath" to
neutralize the excess base. Sodium hydroxide cleans glass by dissolving a tiny layer of
silica, to give soluble silicates. Care should be taken using strongly alkaline solutions to
clean fritted glassware, as this will degrade the frit over time.

- More aggressive methods involving aqua regia (for removing metals from frits),
piranha solution and chromic acid (for removing organics), and hydrofluoric acid baths
are generally considered unsafe for routine use because of possible explosions and the
corrosive/toxic materials involved.

- Chromic acid is not a preferred method if the glassware is to be used for the biological
sciences, as chromate ions can implant themselves in the glass and produce anomalous
results when it is subsequently used for cell cultures; to which the ions are toxic.
A proprietary alternative known as No Chromix is available, which is essentially
a sachet of largely ammonium persulfate and a smaller amount of surfactant. This is
poured into a bottle of concentrated sulfuric.

- Like concentrated hydrogen peroxide, ammonium and sodium persulfate are strong
oxidisers, yet they are not hydroscopic and are more stable. This allows them to be
more easily stored and used. When mixed with concentrated sulfuric, they begin
releasing oxygen, which can oxidize the carbonaceous dehydration products formed
from organic residues by the sulfuric to carbon dioxide; 'burning' them off the glass,
allowing more time for deposits to mechanically break up and for the mixture to be
used before fully decomposing.

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Laboratory Chemicals and Reagents

Chemical substances, materials which can be produced or used in chemical processes.

Chemical processes include such reactions as combustion. Since the rise of the modern
chemical industry in the nineteenth century, numerous chemical substances have been
developed and created including acids, bases, fertilizers, ceramics, catalysts, dyestuffs,
fabrics, explosives, paints, plastics, petrochemicals, pharmaceuticals, agricultural chemicals,
specialty chemicals, automotive materials, home, and commercial electronics components.

In chemistry, a chemical substance is a form of matter that has constant chemical

composition and characteristic properties. It cannot be separated into components by
physical separation methods, i.e. without breaking chemical bonds. They can be solids,
liquids or gases. Chemical substances are often called 'pure' to set them apart from mixtures.
A common example of a chemical substance is pure water; it has the same properties and
same ratio of hydrogen to oxygen whether it is isolated from a river or made in a laboratory.

Other chemical substances commonly encountered in pure form are diamond (carbon),
gold, table salt (sodium chloride) and refined sugar (sucrose). However, simple or seemingly
pure substances found in nature can in fact be mixtures of chemical substances. For
example, tap water may contain small amounts of dissolved sodium chloride and compounds
containing iron, calcium and many other chemical substances.

Chemical substances exist as solids, liquids, gasses, or plasma and may change between
these phases of matter with changes in temperature or pressure. Chemical reactions convert
one chemical substance into another. Forms of energy, such as light and heat, are not
considered to be matter, they are not "substances" in this regard.

Chemical substances (also called pure substances) are often defined as "any material
with a definite chemical composition". According to this definition a chemical substance can
either be a pure chemical element or a pure chemical compound. However, there are
exceptions to this definition; a pure substance can also be defined as a form of matter that
has both definite composition and distinct properties.

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A pure chemical compound is a chemical substance that is composed of a particular

set of molecules or ions. Two or more elements combined into one substance through
a chemical reaction form a chemical compound. All compounds are substances, but not all
substances are compounds.

A chemical compound can be either atoms bonded together in molecules or crystals in

which atoms, molecules or ions form a crystalline lattice. Compounds based primarily on
carbon and hydrogen atoms are called organic compounds, and all others are called
inorganic compounds. Compounds containing bonds between carbon and a metal are called
organometallic compounds. Compounds in which components share electrons are known
as covalent compounds. Compounds consisting of oppositely charged ions are known as
ionic compounds, or salts.

In organic chemistry, there can be more than one chemical compound with the same
composition and molecular weight. Generally, these are called isomers. Isomers usually
have substantially different chemical properties, may be isolated and do not spontaneously
convert to each other. A common example is glucose vs. fructose. The former is an
aldehyde, the latter is a ketone. Their interconversion requires either enzymatic or acid-base
catalysis. However, there are also tautomers, where isomerization occurs spontaneously,
such that a pure substance cannot be isolated into its tautomers. A common example is
glucose, which has open-chain and ring forms.

For industries, chemical includes a wider class of substances that contain many
mixtures of such chemical substances, often finding application in many vocations.
In countries that require a list of ingredients in products, the "chemicals" listed would be
equated with "chemical substances". Within the chemical industry, manufactured
"chemicals" are chemical substances, which can be classified by production volume into
bulk chemicals, fine chemicals and chemicals found in research only.

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Bulk chemicals produced in large quantities, usually with highly optimized continuous
processes and to a relatively low price. Bulk chemicals are usually much less complex.

Fine chemicals produced at a high cost in small quantities for special low-volume
applications such as biocides, pharmaceuticals and specialty chemicals for technical
applications. Fine chemicals may be more complex, many of them simple enough to be sold
as "building blocks" in the synthesis of more complex molecules targeted for single use.

Research chemicals are produced individually for research, such as when searching for
synthetic routes or screening substances for pharmaceutical activity. In effect, their price per
gram is very high, although they are not sold. The cause of the difference in production
volume is the complexity of the molecular structure of the chemical.

The production of a chemical includes not only its synthesis but also its purification to
eliminate by-products and impurities involved in the synthesis. The last step in production
should be the analysis of batch lots of chemicals in order to identify and quantify the
percentages of impurities for the buyer of the chemicals.

Nearly 85% of pharmaceutical products in use require the use of chlorine in their
production. As a result of the chemicals used in pharmaceuticals, combination drug therapy
reduced AIDS deaths by more than 70% from 1994 to 1997. Chemicals called “phthalates”
(there are several kinds of phthalates) are used in polyvinyl chloride (PVC), a vinyl used for
medical tubing, blood bags, and numerous other products. While environmentalists have
tried to ban these products, vinyl medical devices provided numerous lifesaving benefits.

PVC is a safe, durable, sterile product that can withstand heat and pressure, as well as
produce tubing that doesn’t kink. It is particularly beneficial for vinyl blood bags because it
stores blood twice as long as the next best alternative and doesn’t break as glass alternatives
do. With blood shortages looming, PVC blood bags are an essential tool in maintaining and
transporting supplies.

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Modern farming with the proper application of chemical substances, such as chemical
fertilizers and pesticides (herbicides, fungicides, fumigants, rodenticides, insecticides, and
weedicides), provides the benefits of more food production to meet the challenges of the
outpaced population growth. Modern farming provides people in both developed and
developing countries with more food per capita. Herbicides control weeds, reduce the need
for tilling soil, and reduce soil erosion.

Global Regulations of Chemicals: Global advances in researches, technology and

development, identification and formulations of newer chemical products for societal
development, for the improvement of the quality of life along with economic development
have created newer avenues and opportunities. This has necessitated a science-based
regulatory system for the management of chemical substances and to make decisions to meet
the global regulatory challenges.

In this direction, international collaborations and partnerships, have enhanced newer

scientific innovations and greater mobility of a variety of products around the world. This
also has provided increased speed to communicate and share the benefits of technology
between governments.

The data requirements for the registration and distribution of chemical substances, such
as pesticides, drugs and pharmaceuticals, cosmetics, and food products, have been made
uniform. There are many regulatory agencies associated with the safe management of
chemical substances in both developed and developing countries.

Grade of Chemicals: Most, but not all, chemicals are labeled with a grade. The grade
indicates how pure the chemical is. The greater the quantity of other chemicals, metals,
water, or other impurities in the chemical, the lower the grade. There are many different
grading standards, but the three you are most likely to encounter are: reagent grade,
laboratory grade, and technical grade.

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Chemistry Grade Purity Uses

Highest purity available; meets or Works for all scientific and manufacturing
Reagent ACS exceeds standards set by the American needs. Often required for experiments
Chemical Society (ACS) involving living biological matter

Sufficiently pure for most science fair

Relatively high purity, but may contain
Laboratory Lab projects. Not suitable for use in food or
small amounts of impurities
medicine of any kind

Used for commercial or industrial purposes.

Can still be used for many science fair
Technical Industrial Contains impurities
projects. Not suitable for use in food or
medicine of any kind

Manufacturing pure chemicals can be time-consuming and expensive; for this reason,
higher-grade chemicals cost more than lower-grade chemicals. For the purposes of most
science fair projects, laboratory- or technical-grade chemicals are of sufficient purity.

Some chemicals have common household uses either in beauty and hygiene, laundry
and cleaning, building maintenance, or gardening. These chemicals can be bought from local
stores rather than ordered from specialty companies. Unlike chemicals bought from
chemical supply companies, when bought locally these common chemicals are unlikely to
come with Safety Data Sheets (SDS). For general information about handling chemicals. For
specific information about how to handle and dispose of these chemicals.

There are wide range of products of chemicals with most common grading available on
each item. Several quality denominations are common to all manufacturers but, in addition,
every manufacturer creates its own quality denominations for specific applications. The
purity levels and physical and chemical values indicated for the products in this catalogue
represent typical values. Peptide and DNA synthesis: The most important features of these
products are low UV absorption and low water content.

Chemical Abstracts Service (CAS), a division of the American Chemical Society, is the world's leading source of chemical information.
A CAS Registry Number is separated by hyphens into three parts, the first consisting of up to 7 digits, the second consisting of two digits,
and the third consisting of a single digit serving as a check digit. The check digit is found by taking the last digit times 1, the previous
digit times 2, the previous digit times 3 etc., adding all these up and computing the sum modulo 10. For example, the CAS number of
water is 7732-18-5: the checksum 5 is calculated as (8×1 + 1×2 + 2×3 + 3×4 + 7×5 + 7×6) = 105; 105 mod 10 = 5.

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Labeling of Chemicals: Do not remove or deface any existing labels on incoming

containers of chemicals and other materials. The label usually includes the name of the
chemical and any necessary handling and hazard information. Inadequate labels on older
containers should be updated to meet current standards.

To avoid ambiguity about chemical names, many labels carry the CAS registry number
as an unambiguous identifier and this information should be added to any label that does not
include it. On receipt of a chemical, the manufacturer’s label is supplemented by the date
received and possibly the name and location of the individual responsible for purchasing the
chemical. If chemicals from commercial sources are repackaged into transfer vessels, the
new containers should be labeled with all essential information on the original container.

The overriding goal of prudent practice in the identification of laboratory chemicals is

to avoid abandoned containers of unknown materials that may be expensive or dangerous to
dispose of. The contents of all chemical containers and transfer vessels, including, but not
limited to, beakers, flasks, reaction vessels, and process equipment, should be properly
identified. The labels should be understandable to trained personnel and members of well-
trained emergency response teams.

Labels or tags should be resistant to fading from age, chemical exposure, temperature,
humidity, and sunlight. Chemical identification and hazard labels on containers used for
storing chemicals should include following information:
- Identity of the owner,
- Chemical identification and identity of hazard component(s), and
- Appropriate hazard warnings.

Materials transferred from primary (labeled) bulk containers to transfer vessels (e.g.,
safety cans and squeeze bottles) should be labeled with chemical identification and
synonyms, precautions, and first-aid information. Label containers in immediate use, such as
beakers and flasks, with the chemical contents. All reactants should be labeled with enough
information to avoid confusion between them.

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Labeling all containers of experimental chemical materials is prudent. Because the

properties of an experimental material are generally not completely known, do not expect its
label to provide all necessary information to ensure safe handling.

The most important information on the label of an experimental material is the name of
the researcher responsible, as well as any other information, such as a laboratory notebook
reference, that can readily lead to what is known about the material. For items that are to be
stored and retained within a laboratory where the properties of materials are likely to be well
understood, only the sample identification and name are needed.

Recycling of Chemicals: Chemical recycling takes many forms. In each case a

material that is not quite clean enough to be used as is must be brought to a higher level of
purity or changed to a different physical state. Recycling occurs on-site or off-site. On-site
recycling occurs at the laboratory or at a central location that collects recyclables from
several laboratories. Because on-site recycling can be very time and energy intensive, it may
not be economically justifiable.

In some cases, although the amount of waste may be quite small, it can require very
expensive disposal if a commercial vendor must be used. Before a decision on recycling is
made, the cost of avoided waste disposal should be calculated. Because of the difficulty of
maintaining the needed level of cleanliness and safety, on-site recycling of mercury and
other toxic metals is no longer recommended.

Another significant issue is whether recycling activities require a waste treatment

permit under the Resource Conservation and Recovery Act (RCRA). Local regulations must
also be considered. Off-site commercial firms recycle, reclaim, purify, and stabilize vacuum
pump oil, solvents, mercury, rare materials, and metals.

The Resource Conservation and Recovery Act (RCRA), enacted in 1976, is the principal Federal law in the
United States governing the disposal of solid waste and hazardous waste.

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Off-site recycling is preferable to disposal, and sometimes is less expensive. Another

off-site option is to work with suppliers of laboratory chemicals who accept return of
unopened chemicals, including highly reactive chemicals. Gas suppliers sometimes accept
returns of partially used cylinders.

A general comment applicable to all recycling is that a recyclable waste stream needs to
be kept as clean as possible. If a laboratory produces a large quantity of waste xylene, small
quantities of other organic solvents should be collected in a separate container, because the
distillation process gives a better product with fewer materials to separate.

Solvent Recycling: Because the choice of a distillation unit for solvent recycling is
controlled largely by the level of purity desired in the solvent, know the intended use of the
redistilled solvent before equipment is purchased. A simple flask, column, and condenser
setup may be adequate for a solvent that will be used for crude separations or for initial
glassware cleaning.

For a much higher level of purity, a spinning band column is probably required. Stills
with automatic controls that shut down the system under conditions such as loss of cooling
or overheating of the still pot are highly recommended, because they enhance the safety of
the distillation operation greatly. Overall, distillation is likely to be most effective when
fairly large quantities (roughly 5 L) of relatively clean single-solvent waste are accumulated
before the distillation process is begun.

Recycling Containers, Packaging, and Lab ware: Laboratory materials other than
chemicals, such as containers or packaging materials and parts of laboratory instruments,
can also be recycled. Examples include certain clean glass and plastic containers, drums and
pails, plastic and film scrap, cardboard, office paper, light bulbs, circuit boards, other
electronics, and metals such as steel and aluminum. Note that an empty container may still
be subject to management requirements.

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Laboratory Compressed Gases (Cylinders)

In the event of the release of a corrosive gas (e.g. chlorine) or gases that are absorbed
through the skin (e.g. hydrogen cyanide), a complete chemical resistant suit and a self-
contained breathing apparatus are required. There is no practical means of absorbing or
neutralizing a gas, leak must be corrected at the source. Compressed gases are hazardous due
to the high pressure inside cylinders. Knocking over an unsecured, uncapped cylinder of
compressed gas can break the cylinder valve; the resulting rapid escape of high pressure gas
can turn a cylinder into an uncontrolled rocket or pinwheel, causing serious injury and
damage. Poorly controlled release of compressed gas in the laboratory can burst reaction
vessels, cause leaks in equipment and hoses or result in runaway chemical reactions.
Compressed gases may also have flammable, oxidizing, dangerously reactive, corrosive or
toxic properties. Inert gases such as nitrogen, argon, helium and neon can displace air,
reducing oxygen levels in poorly ventilated areas and causing asphyxiation.

Safe handling, storage and transport of compressed gas cylinders

- All gas cylinders, full or empty, should be securely supported using suitable racks,
straps, chains or stands.
- When cylinders are not in use or are being transported, remove the regulator and attach
the protective cap.
- An appropriate cylinder cart should be used for transporting cylinders. Chain or strap
the cylinder to the cart.
- Verify that the regulator is appropriate for the gas being used and the pressure being
delivered. Do not rely upon the pressure gauge to indicate the maximum pressure
ratings; check the regulator's specifications.
- Do not use adaptors or Teflon tape to attach regulators to gas cylinders.
- Never bleed a cylinder completely empty; leave a residual pressure.
- Do not lubricate the high-pressure side of an oxygen regulator.
- Do not expose cylinders to temperature extremes.
- Store incompatible classes of gases separately.

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 Cryogenic hazards

Cryogenics are very low temperature materials such as dry ice (solid CO 2) and liquefied
air or gases like nitrogen, oxygen, helium, argon and neon. The following hazards are
associated with the use of cryogenics:
- Asphyxiation due to displacement of oxygen (does not apply to liquid air and oxygen)
- Embrittlement of materials from extreme cold
- Frostbite
- Explosion due to pressure build up
- Condensation of oxygen and fuel (e.g. hydrogen and hydrocarbons) resulting in
explosive mixtures

The following are precautions for handling cryogenics:

- Control ice build up
- Use only low-pressure containers equipped with pressure-relief devices.
- Protect skin and eyes from contact; wear eye protection and insulated gloves.
- Use and store in well-ventilated areas.
- Keep away from sparks or flames.
- Use materials resistant to embrittlement (e.g. latex rubber tubing).
- Watches, rings, bracelets or other jewelry that could trap fluids against flesh should not
be worn when handling cryogenic liquids
- To prevent thermal expansion of contents and rupture of the vessel, do not fill
containers to more than 80% of capacity.
- If cryogens must be transported by elevator, take adequate precautions to prevent
possible injury. Send cryogenic liquid tanks in elevators without any passengers and
ensure that nobody gets on the elevator while the cryogen is being transported.

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Laboratory Environmental Considerations

Environmental effects are often underestimated during preliminary planning. Dust or

fumes entering the laboratory each time the door is opened, for example, will certainly
create trouble, as will high temperatures in the area adjacent to the laboratory.

Vibration. A less obvious problem than dust, fumes, or heat is vibration, which may
cause difficulties with some types of laboratory equipment, such as analytical balances.
Vibration can also interfere with microscopic work, particularly if this is combined with
photography. In industrial plants, operation of heavy equipment may cause considerable
vibration and should be considered when laboratory location is determined.

One research laboratory was located on the second floor of a building in which a diaper
laundry occupied the first floor. The laundry equipment would periodically send veritable
shock waves through the building, making many laboratory operations impossible for a short
while. The laboratory workers referred to these annoying incidents as the times when the
laundry "dropped its load."

Possible vibration sources outside the building, such as nearby railroad tracks, should
be considered also. In a new testing laboratory, heavy truck traffic immediately outside
caused periodic vibration problems, even though the building sat on a solid concrete slab.
Had this laboratory been on an upper floor, the vibration would have been even more severe.

Sunlight. There is always a question of whether or not a laboratory should have

windows. Windows take up valuable wall space, always at a premium, and should not be
counted on for providing effective ventilation. While sunlight may be a good morale booster
for workers and assist in keeping building warm on cold days, it is at best a nuisance when it
shines on work benches. If there are windows, they should preferable face north or east.

Noise is another environmental factor to be considered. It does not have to be very loud
to seriously affect worker performance if it is persistent. Source of noise disturbance may be
one of much things-plant equipment, heavy traffic outside, ventilation fans, etc.

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Laboratory Safety Considerations

 Why is safety important?

In disputes over location, safety makes an impressive argument. For distance, there
must be a safe exit through parts of the building where is not likely to develop.
Unfortunately, this rule is not always followed in industrial laboratories. Consider the
industrial laboratory which had only one door and no windows. As if this were not enough
of a safety violation, the door was directly across a narrow hall from the boiler room door.
A boiler accident in this building could have entombed the laboratory staff. It is hard to
believe this layout was designed by an architect and approved by local building authorities
in the 1950's. While such a design would be unlikely to be approved today, small industrial
laboratories are still sometimes installed without a proper permit. Such installations often
violate safety rules with respect to both location and layout.

Efficiency Needs: Ease of communication between the laboratory and other areas is
important to consider. There should not be a long hike to the office, processing area, or other
parts of the building with which the laboratory has frequent contact. In one newly built plant,
samples had to be carried down two flights of stairs via heavy doors at each end, across
a busy production area, through another fire door, and finally to the laboratory. Impractical?
Of course. Yet this layout was made by a reputable engineering company with long
experience in the industrial field. Better communication between the designer and a
knowledgeable company representative could have avoided this inefficient plan. In another
plant, the industrial laboratory was installed close to the processing area down a short flight
of stairs. Before this location was chosen, possible hazards and environmental effects were
studied. Here it took little over one minute to bring samples to the laboratory or for
laboratory personnel to be on hand to investigate manufacturing problems.

Fume Hoods space requirements are substantial, since so many off staff need a hood at
the same time. Many operations that used to be performed on the bench must now be done in
a hood for safety reasons.

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 Laboratory Safety

Over the past century, chemistry has increased our understanding of the materials as
well as our ability to work with it. As a result, most of the items we take for granted in
modern life involve synthetic or natural chemical processing.

We acquire that understanding, carry out those manipulations, and develop those items
in the chemical laboratory; consequently, we also must monitor and control thousands of
chemicals in routine use. Since the age of alchemy, laboratory chemicals have demonstrated
dramatic and dangerous properties. Some are insidious poisons.

During the “heroic age” of chemistry, martyrdom for the sake of science was
acceptable, according to an 1890 address by the great chemist August Kekulé: “If you want
to become a chemist, so Liebig told me, when I worked in his laboratory, you have to ruin
your health. Who does not ruin his health by his studies, nowadays will not get anywhere in
Chemistry” Today that attitude seems as ancient as alchemy. Over the years, we have
developed special techniques for handling chemicals safely.

Institutions that sponsor chemicals hold themselves accountable for providing safe
working environments. Local, state, and federal regulations codify this accountability.
Beyond regulation, employers and scientists also hold themselves responsible for the well-
being of building occupants and the general public.

Development of a “culture of safety” with accountability up and down the managerial

(or administrative) and scientific ladders has resulted in laboratories that are, in fact, safe
and healthy environments in which to teach, learn, and work. Injury, never mind
martyrdom, is out of style.

A strong culture of safety within an organization creates a solid foundation upon which
a successful health and safety program can be built. As part of that culture, all levels of the
organization (i.e., administrative personnel, scientists, technicians) should understand the
importance of minimizing the risk of exposure to hazardous materials and should work

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together toward this end. In particular, personnel should consider the health, physical, and
environmental hazards of the chemicals that will be used when planning a new experiment
and perform their work in a prudent manner.

However, the ability to accurately identify and assess hazards is not a skill that comes
naturally, and it must be taught and encouraged through training and ongoing organizational
support. A successful health and safety program requires a daily commitment from everyone
in organization, and setting a good example is best method of demonstrating commitment.

All chemical exposures have the potential for health consequences. Depending on the
toxicology and concentration, the effects of chemical exposures may be immediate (acid
burns) or long term (chronic beryllium disease or cancer). In any case, chemical exposures
may result in life threatening outcomes.

Chemicals may cause physical damage such as explosions or fires resulting in serious
injury and facility damage. Facility and mission related effects might include corrosive
actions that degrade equipment performance and residual contamination that limits the future
use of facilities and equipment.

Environmental issues may arise as a result of spills, releases, or waste chemical

inventories. In addition to the health effects, physical damage, or environmental effects that
may result from a chemical incident, there will be a need to apply scarce resources to
incident mitigation.

For personnel who plan tasks involving chemicals, the goal is to ensure that safety
documentation for the facility, procedures for conducting the task, and supporting hazard
identification and analysis adequately address the full range and scope of chemical hazards.

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 Laboratory Safety Responsibilities

The responsibility for the management of laboratory safety and adherence to safe lab
practices rests within units and departments. All personnel, including directors, supervisors,
and employees have a duty to fulfill their obligations with respect to maintaining a healthful
and safe work environment.

Laboratory Directors are responsible to:

- Ensure that activities conducted within their area of responsibility comply with
company policies and relevant legal requirements.
- Ensure that all stuff working within their unit are provided sufficient information,
training and supervision to carry out their work safely.
- Ensure that all lab stuff are equipped with the required personal protective equipment
(PPE) and to ensure that such PPE are maintained properly and used correctly.
- Ensure that safety devices and engineering controls are adequate, appropriate, and in
good working order.
- Ensure that all stuff receive appropriate and adequate information and training to be
able to respond to emergency situations.

Laboratory Stuff (personnel) is responsible to:

- Be familiar with the safety instructions, whether written or oral, and to comply with
these instructions when conducting laboratory work;
- Wear the appropriate personal protective equipment when present in the lab and when
conducting work with hazardous materials or operations;
- Report all accidents, dangerous incidents or suspected occupational illnesses to their
immediate supervisor without delay;
- Refrain from manipulating any hazardous materials prior to undergoing appropriate
safety training and receiving safety instructions.

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Laboratory Safety Orientation

All Laboratory Personnel should be provided with a laboratory safety orientation that
includes, but is not limited to, the following:
- Rights under Act Respecting Occupational Health and Safety, with specific emphasis
on: Right to know about workplace hazards and controls; Right to participate in
decisions about their personal health and safety; and Right to refuse unsafe work.
- Emergency procedures;
- Health and safety policies;
- Accident, incident and occupational disease reporting procedures;
- hazards/unsafe conditions reporting procedures;
- Instruction on safe work practices and procedures required to work safely in the
laboratory, work area, facility, or field research placement;
- Description of existing hazards and what controls are in place; and
- Personal protective equipment required to perform work safely.

Laboratory Safety Orientation Procedure

- Laboratory Supervisors Safety Training Requirements of Laboratory Safety Orientation

Checklist for each new Laboratory Personnel;
- Laboratory Personnel receives the Laboratory Safety Orientation Checklist prior to
starting their work, study and/or research and completes the form, attending the
specified safety training;
- The signed Laboratory Safety Orientation Checklist is returned to the Laboratory
Supervisor within one month of the Laboratory Personnel’s arrival;
- Laboratory Supervisors review and sign completed Laboratory Safety Orientation
Checklist, ensuring that all material has been reviewed and safety trained attended;
- Once completed, the Laboratory Safety Orientation Checklist should be retained by the
Laboratory Supervisor for recordkeeping.

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Laboratory Safety Policy

The scientific laboratory is a place of adventure and discovery. Some of the most
important events in scientific history have happened in laboratories. The antibiotic powers of
penicillin were discovered in a laboratory. The plastics used today for clothing and other
products were first made in a laboratory. The list is endless. One of the first things any
scientist learns is that working in the laboratory can be an exciting experience.

However, the laboratory can also be quite dangerous if proper safety rules are not
followed at all times. In order to prepare yourself for a safe work in the laboratory, read over
the following safety rules. Then read them a second time.

Make sure you understand each rule. If you do not, ask your supervisor to explain any
rules you are unsure of. You may even want to suggest further rules in the section labeled
"Other Rules". When you are satisfied that you understand all the rules on this list, sign and
date the contract in the place provided. Signing this contract tells your teacher that you are
aware of the rules of the laboratory.

Stuff on laboratory will be doing many laboratory activities that may require the use of
chemicals, laboratory equipment, and other items which, if used incorrectly, can be
hazardous. Safety in the laboratory is the number one priority for Stuff, Suppervisors, and
Directors. To ensure a safe laboratory, a list of rules has been developed and provided to you
in this stuff safety contract.

These rules must be followed at all times. The laboratory stuff must sign their
copy. Please read the entire contract before you sign. Laboratory stuff will not be allowed in
the laboratory until all their contracts are signed and given to the Director. You can request
an additional hard copy.

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General Rules:

- Follow the written lab procedure - laboratory activity at this level is not meant to be
creative. Improper combinations or amounts of chemicals can be very dangerous. No
unauthorized experiments to be performed. If you curious about trying a procedure not
covered in the experimental procedure, consult with your laboratory instructor.

- When first entering a lab room, do not touch any equipment, chemicals, or other
materials in the laboratory area until you are instructed to do so.

- Never perform activities that are not authorized by your supervisor. Always obtain
permission before "experimenting" on your own.

- OBEY all safety rules

- Never work alone in the laboratory.

- NO smoking, eating or drinking will be permitted in the laboratory.

- Certain products, like hair spray, are flammable and should not be worn while working
near an open flame.

- There should be no loud talking or horseplay in the laboratory.

- Use common sense and do not rush in the laboratory. Never be complacent about
chemicals or chemical reactions.

a) Don’t take chances b) Don’t hurry c) If not sure ASK!

- Read all directions for an experiment several times. Follow the directions exactly as
they written. If you are in doubt about any part of the experiment, ask for assistance.

- As a responsible citizen, be aware of the location of and the procedure for using the
nearest fire alarms, fire-evacuation routes and any other safety equipment, such as fire
blankets and eyewash fountains.

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- Lab tables should be as uncluttered as possible to allow work space and avoid
accidents. Also, keep the aisles clear to prevent tripping over your gear, and so that
other people can pass unhampered. Place book bags, pocketbooks, under lab tables.

- Lab activities require your undivided attention. No music allowed in labs. Radios
(including Walkman type) and other entertainment devices are not permitted. No
cellular phone use.

- Computers are for laboratory business only - no Internet surfing.

- Wash your hands before leaving the lab and do not eat in the lab.

- Keep your work space clean and tidy. The working space, desk drawers, cabinets, lab
equipment and instruments must be kept neat and clean at all times. Clean your work
area before leaving! Follow your supervisor directions for washing, unplugging and
putting away the equipment. Wash hands with soap and water after working in the
laboratory.

- Properly label all materials to be used in the experiment. Label all Petri dishes and test
tubes to be incubated with the date, your name, experiment number and organism (if
known) and place in the basket provided. Any unlabeled items will be discarded.

- Wear protective gloves or oven mitts to avoid burns.

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Personal Protection Equipment (PPE)

- Wear approved safety goggles when working with or around chemicals, any
mechanical device, or any type of flame or heating device.

- If any substance gets in your eyes or spills or your skin or clothes, rinse it immediately
with water and have someone notify your supervisor.

- Safety glasses face shield, and shoes (no sandals) must be worn in the Lab when
needed. Normal prescription lenses are insufficient!. Other eye/face protection may be
required with specific procedures.

- Contact lenses are discouraged. The safety of wearing contact lenses in laboratories has
been hotly contact lenses can be worn if and only if proper protective eyewear is also
worn. If you choose to wear contacts, please tell your lab instructor.

- Know the location and use of all safety equipment (goggles, aprons, eyewash, fire
blanket, fire extinguishers, etc.)

- Learn where the safety and first-aid equipment is located. This includes fire
extinguishers, fire blankets, and eyewash stations.

- Appropriate gloves will be provided when needed. Use of gloves is required for
handling certain chemicals.

- Gloves are very expensive. Do not change gloves needlessly.

- Appropriate clothing is required. Your clothing is a barrier between your skin and
chemicals. Lab coats are recommended

- Shoes must be worn.

- No sandals, thongs, open toed or open heeled shoes.

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Eye and face protection: All staff, and visitors must wear appropriate eye and/or facial
protection in following :
- All areas where hazardous materials, or substances of unknown nature used or handled
- All areas where possibility of splash, flying objects, moving particles and/or rupture exist
- All areas where there are other eye hazards, e.g. UV or laser light

Instructions for selection and use of protective eyewear are as follows:

- Light-to-moderate work: approved safety glasses with side shields.

- Work with significant risk of splash of chemicals, or projectiles: goggles.
- Work with significant risk of splash on face, or explosion: full face shield, plus goggles.
- If safety glasses with correction lenses are needed, first consult with your optometrist

Foot Protection: Scientists have marveled at the design and structure of the human foot.
Human foot is rigid enough to support the weight of your entire body, Protective footwear
worn in the workplace is designed to protect the foot from physical, and chemical hazards

Lab coats: Appropriate protective clothing (e.g., lab coats, aprons, and coveralls) is
required in all experimental where hazardous materials are handled. Instructions for
selection and use of protective laboratory clothing are as follows:
- Select knee-length lab coats with button or snap closures
- Remove protective clothing when leaving the laboratory
- Remove protective clothing in the event of visible or suspected contamination
- Wear a solid-front lab coat or gown with back closures and knitted cuffs when working
with highly toxic or infectious agents
- Wear protective aprons for special procedures such as transferring large volumes of
corrosive material.

Hand protection: In the laboratory, gloves are used for protection from radiation,
chemical products, biohazardous material and physical hazards such as abrasion, tearing,
puncture and exposure to temperature extremes.

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Respirators: should be used only in emergency situations (e.g. hazardous spills or

leaks) or when other measures, such as ventilation, cannot adequately control exposures.
There are two classes of respirators: air-purifying and supplied-air. The latter supply clean
air from a compressed air tank or through an air line outside the work area, and are used in
oxygen-deficient atmospheres or when gases or vapors with poor warning properties are
present in dangerous concentrations. Air-purifying respirators are suitable for many
laboratory applications and remove particulates (dusts, mists, metal fumes etc.) or gases and
vapors from the surrounding air.

Selection, use and care of respirators

Follow proper procedures for selecting and using respiratory protective equipment.
Correct use of a respirator is as vital as choosing the right respirator. An effective program
for respiratory protection should include the following:
- Selecting a respirator that is suitable for the application.
- Assigning respirators to individuals for their exclusive use, whenever possible.
- Evaluation of facial fit for all users of respirators; beards, long sideburns, glasses or
wrong size of respirator may prevent an effective seal.
- Protocols for using, cleaning and sanitary storage of respirators.
- Regular inspection of the respirator, and replacement of defective parts

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Handling and Storage of Chemicals

Storing chemicals in stockrooms and laboratories requires consideration of a number of

health and safety factors. In addition to the inventory control and storage area considerations
discussed above, proper use of containers and equipment is crucial. In addition to the basic
storage area guidelines above, follow these general guidelines when storing chemicals:
- Label all chemical containers appropriately to ensure that chemicals stored safely.
- Place user’s name and date received on purchased materials to inventory control.
- To avoid clutter, avoid storing chemicals on bench tops, except for those chemicals
being used currently.
- To avoid clutter and to maintain adequate airflow, avoid storing chemicals in
chemical hoods, except for those chemicals in current use.
- To assist in maintaining a clean work environment and to ensure that segregation of
incompatible chemicals is maintained, provide a definite storage place for each
chemical and return the chemical to that location after each use.
- Store volatile toxic or odoriferous chemicals in a ventilated cabinet. Check with the
institution’s environmental health and safety officer.
- Provide ventilated storage near laboratory chemical hoods.
- If a chemical does not require a ventilated cabinet, store it inside a closable cabinet
or on a shelf that has a lip to prevent containers from sliding off in the event of
a fire, serious accident, or earthquake.
- Do not expose stored chemicals to heat or direct sunlight.
- Observe all precautions regarding the storage of incompatible chemicals.
- Separate chemicals into compatible groups and store alphabetically within
compatible groups. Because chemicals in storage are contained, their separation by
compatibility groups can be simplified.
- The color coded system allows for ease of storage.
- Store flammable liquids in approved flammable liquid storage cabinets.
- Consider the security needs for the materials.

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Safety Data Sheets (SDS)

A Safety Data Sheets (SDS) provide more details than labels. They are technical
bulletins that provide chemical, physical, and toxicological information about each
controlled product, as well as information on precautionary and emergency procedures. They
must be readily accessible to anyone who works with, or who may otherwise be exposed to,
controlled products.

A safety data sheet (SDS) is a form containing data regarding the properties of
particular substance. An important component of product stewardship and workplace safety,
it is intended to provide workers and emergency personnel with procedures for handling or
working with that substance in a safe manner, and includes information such as physical data
(melting point, boiling point, flash point, etc.), toxicity, health effects, first aid, reactivity,
storage, disposal, protective equipment, and spill handling procedures. The exact format of
an SDS can vary from source to source within a country depending on how specific is the
national requirement.

Everyone has the right to review an SDS, whether it is related to their work, or simply
because of personal interest.

Suppliers controlled products are required to make available SDS to the purchaser. The
SDS must be available in both official languages. Should any new information arise about
product, the Supplier is required to revise the SDS.

" Safety Data Sheet for a controlled product shall be kept at the workplace by the employer
in place that is known to the workers and shall be easily and rapidly accessible to those
workers that are liable to come into contact with the product. That data sheet shall be in
the form of document that is easy to handle and consult."

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International Chemical Safety Cards

Right-To-Know Wallet Cards RTK Safety

NFPA chemical safety labeling

HEALTH (BLUE)

4 Danger Fatal on short exposure. Specialized protective equipment required

3 Warning Corrosive or toxic. Avoid skin contact or inhalation

2 Warning May be harmful if inhaled or absorbed

1 Caution May be irritating

0 - No unusual hazard

FLAMMABILITY (RED)

4 Danger Flammable gas or extremely flammable liquid

3 Warning Flammable liquid flash point below 100° F

2 Caution Combustible liquid flash point of 100° to 200° F

1 - Combustible if heated

0 - Not combustible

REACTIVITY (YELLOW)

4 Danger Explosive material at room temperature

3 Danger Explosive if shocked, heated or mixed with water

2 Warning Unstable or may react violently if mixed with water

1 Caution May react if heated or mixed with water but not violently

0 Stable Not reactive when mixed with water

SPECIAL WARNINGS (WHITE)

W - Water Reactive

Oxy - Oxidizing Agent

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Risk and Safety Statements, also known as R/S statements, R/S numbers, R/S
phrases, and R/S sentences, is a system of hazard codes and phrases for labeling dangerous
chemicals and compounds. The R/S statement of a compound consists of a risk part (R) and
a safety part (S), each followed by a combination of numbers. Each number corresponds to
a phrase. The phrase corresponding to the letter/number combination has the same meaning
in different languages—see 'in other languages' on the left.

R-phrases (short for Risk Phrases) "Nature of special risks attributed to dangerous
substances and preparations".

S-phrases (short for Safety Phrases) "Safety advice concerning dangerous substances
and preparations". These safety phrases are used internationally and not just in Europe, and
there is an ongoing effort towards complete international harmonization.

Example: R/S statement code for fuming hydrochloric acid (37%): R: 34-37 S: 26-36-45.
The corresponding English language phrases:

Risks
R: 34 Causes burns
R: 37 Irritating to the respiratory system.

Safety
S: 26 In case contact with eyes, rinse immediately with water and seek medical advice.
S: 36 Wear suitable protective clothing.
S: 45 In case of accident or if you feel unwell, seek medical advice immediately.

Dashes separate the phrase numbers. They are not to be confused with range indicators.

Example: R: 34-37 Causes burns, irritating to the respiratory system.

Slashes indicate fixed combinations of single phrases.

Example: R: 36/37/38 Irritating to eyes, respiratory system and skin.

More detailed hazard and safety information can be found in the material safety data sheets
(MSDS) of a compound

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Flammable & Exposure limits (TLV, PEL)

An exposure limit is maximum limit of exposure to an air contaminant. The threshold

limit value (TLV) or permissible exposure limit (PEL) can be expressed as the following:
- 8-hour time-weighted average (TWA) is average concentration to which most workers
can be exposed during an 8-hour workday, day after day, without harmful effects.
- Short-term exposure limit (STEL), is maximum average concentration to which most
workers can be exposed over a 15-minute period, day after day, without adverse.
- Ceiling (C) defines a concentration that must never be exceeded; and is applied to many
chemicals with acute toxic effects

It should be noted that most exposure limits are based on industrial experiences and are
not entirely relevant to the laboratory environment. Good laboratory practices and well-
designed ventilation systems serve to maintain air concentrations well below these limits.

Flammable limits or explosive limits define the range of concentrations of a material in

air that will burn or explode in the presence of an ignition source such as a spark or flame.
Explosive limits are usually expressed as the percent by volume of the material in air:
- The lower explosive limit (LEL) or lower flammable limit (LFL) is the lowest vapour
concentration that will burn if ignited. Below this limit, the concentration of fuel is too
"lean" for ignition, i.e., mixture is oxygen rich but contains insufficient fuel.
- The upper explosive limit (UEL) or upper flammable limit (UFL) is highest vapour
concentration that will ignite. Above this limit, the mixture is too "rich" for ignition.
- The flammable range consists of concentrations between the LEL and UEL

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Waste Collection and Disposal

The laboratory operator must make a careful examination of all wastes that will be
generated and, from this, work up a waste disposal system. Some wastes may be compatible
and could be disposed of together. Others could react and thus cause problems. Flammables
must be given special attention.

Certain biological wastes may be very hazardous even in small quantities. Special rules
apply to radioactive materials, even in the small amounts used for investigative purposes.
Disposal Containers In the laboratory, wastes are collected in suitable containers placed in
convenient locations. Kneeholes in work benches are good for this purpose, since the
containers are then out of the way. Waste containers must be compatible with that is put into
them. Acidic materials, for instance, may quickly damage steel buckets. Some plastics may
not stand up to solvents placed in them, and so on.

Flammables must go into approved safety cans. Dry waste should be put into self-
closing containers designed to snuff out a possible fate. Lining solid waste containers with
plastic bags is highly recommended. All containers must be clearly marked as to contents.
Color coding with wide adhesive tape is one way to do this. Special warnings should be
placed on containers for particularly hazardous materials. A typical example of poor waste
management reported in the press concerned an unmarked waste container in a university
laboratory. When the container showed signs of heat-producing reaction and began to leak,
a professional cleanup team was called in. Although only four gallons of material was
involved, 27 different chemicals were identified in the mixture!

Waste Disposal Services: There are no any companies specializing in Taste disposal.
Local ones are listed in the yellow pages of the telephone directory. The laboratory operator
should contact more than one for suggestions and estimates. In such discussions, a disposal
service rill asks detailed questions as to the exact nature of the waste and quantities
involved. An agreement will be made about the types of shipping containers to be used.
These are non returnable.

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The disposal service may sell suitable containers and require these for certain types of
waste. In other cases, the laboratory may provide its own. If drums are needed, they are
available from companies engaged in drum reconditioning. Manufacturers of chemicals may
have used drums available at reasonable prices, but since these will contain residues of their
former contents, a check for compatibility must be made before using them.

Waste Storage: It is important to keep the amount of potentially hazardous waste in the
laboratory to a minimum at all times. Periodically, contents of the laboratory waste
containers will be transferred to appropriate containers for final disposal. These must be
stored in a safe location, often outdoors, while awaiting pick-up by a disposal service. There
will be local restrictions for such storage. A locked storage area may be needed, for
example, to prevent unauthorized access to hazardous materials. The fire department may set
strict limits as to how much flammable material may be present. All containers must be
marked with contents, and the storage area will no doubt require warning signs.

Solid Waste: Whatever goes to local sanitary dump will eventually find its way into
the environment. For this reason, materials that are to be disposed of as garbage from the
laboratory should be carefully scrutinized. There are those who feel that traces of hazardous
materials when mixed with large amounts of regular garbage will somehow disappear. They
will not. Worse yet, some materials could react when combined and possibly generate
enough heat to cause fire. Broken glassware free from hazardous chemicals, paper towels,
empty containers that have not held toxic, flammable, or highly reactive chemicals are all
good candidates for the garbage container.

For any other waste material, the laboratory operator has to make decisions. Filter
paper, for instance, could contain residue that should not be disposed of as garbage.
Anything that contains heavy metals or ionic species that may be termed hazardous must be
given special disposal. Same is true for both organic and inorganic materials from which
natural processes, such as leaching, could extract hazardous substances.

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Old Chemicals: Any laboratory that has been in operation for some years will have
a collection of old chemicals purchased for past projects, which may have been completed or
just abandoned. Even though they take up valuable storage space, there is a feeling that they
may be useful some day.

Over time, however, some reagents may have picked up enough moisture to be
transformed from free-flowing powders to rock-hard substances containing unknown
amounts of water of crystallization.

Others may have hydrolyzed to a point where the original analysis is meaningless. Heat
and light may have caused some to break down, and a few may have become dangerous. For
example, a half-filled can of ethyl ether that has been sitting on the shelf for an extended
period of time is best handled like a potential bomb. Periodic inventory of chemicals stored
in the laboratory is therefore very much in order.

Since pollution control and waste disposal problems vary greatly from one laboratory to
another, they have to be handled on a custom basis. The laboratory operator will no doubt be
an expert on the materials used but not on their disposal. It is important for him to stay in
touch with people familiar with disposal and provide them with detailed information.
Industrial laboratories often handle a relatively limited number of chemicals. Since many of
these same chemicals are also used on a manufacturing scale, their disposal will have
already been planned for by plant personnel.

Disposal of chemicals used only in the laboratory, however, for investigative and
development purposes must also be considered, as well as reagents used for testing.
Laboratories handling biologicals have their own special problems. They often have to
dispose of small but significant amounts of materials that may be very hazardous. Every
laboratory procedure must then be scrutinized with this in mind.

Sinks and Drains: Do not flush any hazardous waste materials down the sink drains.
Do not pour any waste solids in the sinks that may clog drains. Do not remove strainers from
sink drains. Clean the strainers as necessary to maintain good drainage.

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Spills and spill control

No liquid waste can be disposed of directly into the environment or into a storm sewer
system. Unless collected and handed over to a waste disposal company, it goes into the
sanitary sewer. There are specific rules concerning the quality of what may be disposed of in
this manner. Materials that are routinely sent to the sewer from a home may not be
permissible from a commercial source. Normally accepted waste water rules are often made
more restrictive by local ordinance. Waste water rules have pH limits, a common range
being between 6 and 10. There are also limits for fats and oils, solvents, heavy metals, and
a variety of other compounds and ions.

The fact that a compound with possible toxic or otherwise undesirable properties is
not on the list does not mean it is permissible. Such a matter should be discussed with the
proper authorities. The discharged water may also have to pass a test for toxicity to aquatic
animals. As one frustrated manager of a chemical plant put it: "We can no longer put
anything but pure tap water into the sewer!" Of course, it is not really that bad, but some of
the requirements often come as a surprise. Waste water rules sometimes require that water
conform to the limitations at all times. Under such rules, surges of non-conforming
sewage are not permitted.

Hazardous chemical spills: In the event of a spill of a hazardous (volatile, toxic,

corrosive, reactive or flammable) chemical, the following procedures should be followed:
 If there is fire, pull the nearest alarm. If you are unable to control or extinguish a fire,
follow the fire evacuation procedures
 If the spill is in a laboratory, shop or chemical storeroom:
o Evacuate all personnel from the room
o Be sure the hood/local exhaust is turned on
o If flammable liquids spilled, disconnect electricity to sources of ignition if possible
o Call the campus emergency telephone number to request additional assistance if
you cannot manage the clean-up yourself.

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 If the spill is in a corridor or other public passageway:

o Evacuate all people from the area and close off the area to keep others out.
o Call the emergency telephone number, to have the air system in the area shut down
(to prevent contamination of other areas) and to request additional assistance.

Spill response contingencies: Laboratory heads responsible for predetermining

procedures for response to the types of spill situations that may be anticipated for their
operations. Individuals requiring assistance in preparing spill response plans should contact
Environmental Health, and Safety local phone. In instances where more extensive equipment
or technical assistance is needed, backup can be provided by other internal resources.
Communications are handled through the emergency telephone number.

Development of spill response plans: All laboratories housing hazardous materials are
required to provide means of reaching contact people who may be summoned in the event of
emergencies involving their laboratory, especially for after-hours situations. This may
involve posting the relevant telephone number(s) and/or providing them to the Security
Services, who operate the emergency telephone number. Building Directors are also
required to provide to the Security Services telephone numbers where they, or alternate
contact persons, may be reached during after-hours crises

Chemical Spill Kits: Each laboratory has a unique composition of hazardous and non-
hazardous chemicals in various states. Therefore, spill kit requirements of each laboratory
are also unique. There are general guidelines to follow when deciding how to appropriately
stock a spill kit. Few labs are properly equipped without supplementing the basic spill kit
with items that meet the specific needs of that laboratory.

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Emergency Planning for Laboratories

In an effort to support the laboratory, the Health and Safety Office has developed
Emergency Plans to update critical information needed in the plans. Also included are
procedures for many different types of emergency situations. General emergency
procedures were developed by the Health and Safety Office and include step by step
instructions for medical emergencies, fires, hazardous materials spills, radioactive materials
spills, threatening person situations, earthquakes, bomb threats and electrical failure.
Individual departments and/or laboratories are encouraged to provide additional information
specific to that organization. It is imperative that faculty, staff are aware of the Department
Emergency Plans and trained on the procedures contained within.

Laboratory equipment, materials and research can be protected from loss during
emergencies, by taking appropriate precautions that will minimize the impact of dangerous
conditions resulting from fire, severe weather, utility failures or loss of services (e.g. electric
power, heat, air conditioning, water, etc.) Prepare a lab contingency plan that meets your
specific needs. This plan should be shared with your lab, your department and your Building
Manager for inclusion in the Building Emergency Plan. The plan should be implemented
whenever a severe weather event has been issued. Remember, you must take responsibility
to protect your laboratory and research.

Before a laboratory can develop an effective plan for responding to emergencies, the
laboratory’s current capabilities must be determined. This would include both diagnostic and
patient support testing capabilities and capacity. An in-depth assessment can be a valuable
tool for the lab to use in advancing its emergency response preparations. Because the clinical
laboratory will often be the first line of response during diverse community emergency
events, the laboratory should consider an “All- Hazards Plan” approach to planning. An All-
Hazards response plan should include procedures for sampling, analysis or referral, and
reporting for biological, chemical, and radiological testing of clinical samples. The plan can
also be adapted for responding to other events that might assail a community, including
natural and accidental disasters.

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Laboratory Equipment and Facilities

The locations of all such equipment item are indicated in the lab directory Equipment
items with property numbers removed from normal storage location for use must be signed
out on the equipment sign out sheet in the chemicals lab. Do not operate equipment or
instruments if you are not familiar with their operation. Read instruction manuals carefully
or consult lab supervisor before using equipment.


The laboratory is built, work benches are in place, and utilities are hooked up. All is
now in readiness to receive the equipment and supplies to begin operation.

Equipment Sources: Laboratory equipment and supplies are available from several
sources, such as laboratory supply houses, manufacturers' representatives, mail order houses,
and local retail stores.

Laboratory Supply Houses: A supply house, which generally represents several

manufacturers, may be nationwide, regional, or local. Many offer a broad range of supplies,
while others specialize in certain fields, such as medicine or education. A supply house
usually has a "will call" desk, where an urgently needed item may be picked up within hours
after the order is placed.

Factory Direct: Much equipment is now sold directly by the manufacturer through
a network of representatives. This is particularly true for high priced instruments. Such items
may also be offered on a lease basis.

Mail Order Companies: Mail order companies often offer excellent service. Their
catalogs sometimes list specialty items not sold elsewhere, such as unique pH electrodes or
plastic products. Both laboratory supply houses and mail order companies may sell popular
types of instruments under their private labels at substantial savings.

Science Shops: Small retail stores called "science shops" are found in many larger
cities. While their prices may be on the high side, they offer over-the-counter service for

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many items needed in a hurry. They will also sell glassware by the piece rather than by the
case, a service often desirable for small laboratories.

Hardware and Electronic Stores: Local suppliers of hardware and electronic parts
often offer many items useful in the laboratory at very competitive prices. Drugstores
and Supermarkets At large drugstore chains and supermarkets, the operator of a laboratory
can found great bargains on items such as paper towels and cleaning products when they
are on special sale.

Where to Obtain Information on Suppliers: Scientific and technical journals carry

advertising by laboratory supply companies. Many have reader service cards that can be
mailed in for further information. Since service may be slow, some of the advertisers have
toll-free phone numbers for quick response to questions.

Local supply houses are listed in the yellow pages in the phone directory. All it takes is
one call, and the sales representative will show up, catalogs in hand. As already mentioned,
tl1e annual Lab Guide, published by the American Chemical Society, is also an excellent
source of information on suppliers.

Selecting Equipment: Selecting equipment for a new laboratory calls for a careful study
of catalogs and many discussions with sales representatives. As a rule, each item considered
will have its good and its less desirable points. Choosing the most suitable model for
a specific laboratory will often involve a compromise.

If a sales representative offers to arrange for a visit to a laboratory where equipment of

the type being considered is in use, such an offer should not be turned down. A discussion
with an actual user will be very fruitful. Some manufacturers show their equipment in
display rooms, giving the prospective buyer a chance for true "hands-on" experience.

Electronic developments have revolutionized many types of laboratory equipment. Few

instruments with dials are seen today, for instance. Digital readouts have taken over. While
easier to use, estimating the amount of fluctuation of unstable signals is more difficult on

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a digital readout. There are also cases where an instrument's readout is more sensitive than
its detection device, thereby causing unstable readings.

For certain applications, a dial instrument may still be preferable. Electronic balances
are now the rule rather than the exception. They are not only easy to use, but they generally
require less service than mechanical ones.

Prices have been considerably reduced in recent years. Power supplies to instruments
have come a long way since the old days of the electron tube. Solid state devices develop
very little heat, which was a problem in older equipment.

However, many solid state devices are sensitive to sudden voltage fluctuations, or they
may suffer damage if the line power fails and suddenly comes on again. Much of the newer
equipment may be connected to data processing systems, very important there a high volume
of work is performed.

Selecting the right equipment has become quite difficult today because of the
tremendous variety available. In addition, the planner must look into the future. Will a
certain piece of equipment be suitable for future work? Here is a typical example: A forward
looking laboratory operator insisted on a pH meter that also could be used for specific ion
determinations, even though such work was not being done at the moment.

It took some time to get management approval for this more expensive instrument, but
within 6 months specific ion determinations were started. A study of catalogs will show new
trends in equipment design, which will soon make older types obsolete, even though they
have not yet been discontinued.

Selecting Supplies: A new laboratory will need a start-up supply of a variety of

consumable items. How much should be purchased? While it may be tempting to buy large
amounts of items such as glassware and reagents while management is still in a spending
mood, it may also be unwise. First of all, there is storage to consider as well as the fact that
many reagents have limited shelf lives. On the other hand, prices at start-up could be very

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favorable, since supplies will come as part of a general bid. Such pros and cons must be
carefully weighed. Note also that management have definite limits on inventory of supplies.

Cost Estimates: Starting up a new laboratory means preparing a long and detailed
shopping list. Everything, down to the smallest spatula and hose connector, must be listed.
This takes time and much attention to detail. For each operation, everything that is needed
should be listed down to the size and type of filter paper. Then the list is consolidated, since
many items are used for more than one kind of work. Sometimes buying a different size or
model of an item will make it do double duty.

What will it cost? A laboratory operator should be very careful about discussing figures
with management until estimates have been made. Prices given in catalogs may not be
current and should always be verified. Possible discounts from regular prices should not be
taken into account unless they are guaranteed. Some instruments may require certain
accessories that are sold separately. One laboratory, for instance, almost overlooked ordering
the ultrasonic cleaner needed for periodic servicing of an instrument component.

In another case, special glassware was needed for the operation of an instrument.
The cost of minor items, such as reagents, glassware, and thermometers, adds up faster than
most planners realize. The idea is to present management with a realistic start-up budget.
Adding items after a budget is approved will involve a good deal of persuasion.

Ordering: The manner in which orders are placed varies from one laboratory to
another. In a large organization, the laboratory operator will prepare a requisition, which
goes to the purchasing department, often via a department head for approval. Copies of the
requisitions should be kept in the laboratory, which should also receive copies of actual
purchase orders. In a small laboratory the operator may do the ordering himself. Obtaining
bids from two or more suppliers is highly recommended for larger orders at start-up.

The prices quoted may come as a pleasant surprise, since a supply house will put its
best foot forward when bidding on equipment for a new laboratory. If they get the business,

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they will have a foot in the door when it comes to orders for future day-to-day supplies,
which are their bread and butter.

Bids should be gone over in detail, not only for correctness, but also for possible
substitution of some items. A laboratory supply house will require credit information before
accepting an order from a new customer. This is generally a simple procedure.

Capital Equipment: As equipment and supplies arrive, the laboratory operator will be
contacted by the accountant, who will want to know which items are to be capitalized and
how they are to be amortized. This is very important for tax purposes. Rapid amortization
will usually offer many advantages, but IRS will question write-offs that seem to be too
quick. Capital equipment is durable and not consumed during operation. In time, of course,
it will suffer wear and tear and eventually become unusable. Its life will also be shortened by
obsolescence, a very important factor.

A 50 year old two-pan analytical balance, for example, may be in perfect working
order, but its value is only that of an antique. The cost of equipment will also determine
whether or not it should be capitalized. Rules for this will vary from one laboratory to
another. It is up to the laboratory operator to estimate the effective life of a piece of
equipment. He must be able to justify such an estimate in case of a challenge from IRS.
This calls for detailed knowledge of the equipment and its use, plus some idea of how soon
it may become obsolete.

Equipment Identification: All laboratory equipment of any appreciable value should

carry some type of identification. This should be arranged for as soon as the equipment
arrives. It is particularly important for capital equipment in order to keep accounting records
straight. Permanently attached metal tags with numbers are often used but may be hard to
attach to some types of laboratory equipment. Smaller items of relatively low value could
also carry some type of identification.

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A number of options may be available for conducting analyses of samples. The agency
responsible for the monitoring programme may have its own laboratory or laboratories, the
facilities of another agency or of a government ministry may be available, or some or all of
the analytical work may be done under contract by a private laboratory. Some analytical
work will inevitably be done in the field, using either field kits or a mobile laboratory.
Regardless of the options chosen, the analytical services must be adequate for the volume of
work expected. Some of the relevant considerations in this context are:

- Variables to be analyzed. If only a few simple tests are required, analyses can be
undertaken in the field using field kits. More complex testing programmes may require
the services of specialized laboratories.
- Sampling frequency and number of sampling stations. The frequency with which
samples must be taken and the number of sampling stations involved will obviously
influence the volume of work necessary and, hence, the staff and facilities required
- Existing laboratory facilities. Laboratory facilities may be under the direct control of
monitoring agency or be associated with another agency (e.g. health ministry, regional
hospital, or a college or university). The major concern is that laboratory is sufficiently
close to the sampling stations to permit samples to be delivered without undue delay.
- On-site testing. Some analyses must be performed in the field. Modern field kits are
available that permit analyses of a wide range of variables. This makes it possible to
run a monitoring programme without the need for a fixed laboratory, but raises certain
problems of analytical quality control.
- Temporary laboratories. If a monitoring programme is expected to be of short duration,
it may be expedient to set up a temporary laboratory. Sufficient space, water and
electricity supplies are essential, but equipment and supplies can be brought in and then
removed after the monitoring programme is completed.
- Mobile laboratories. It is possible to set up a laboratory in a suitable motor vehicle, e.g.
truck or van. In effect, this is a variant of on-site testing, but may provide better
facilities than field kits.

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In practice, the usual arrangement is for the agency responsible for water quality
monitoring to establish its own central laboratory, which can be organized to provide
training and supervision of staff, repair of equipment and various other services. However, if
the monitoring area is large or transportation is difficult, regional laboratories may be set up
or field kits used for certain analyses.

Analyses that require expensive and sophisticated equipment, or that can be undertaken
only by highly trained personnel, are performed only at the central laboratory, for example
analysis for heavy metals using atomic absorption spectrophotometry and analysis for
pesticides and herbicides using gas chromatography.

Laboratory facilities should be clean, temperature and humidity controlled, and have
adequate lighting at bench tops. They should have provisions for disposal of microbiological
waste. Laboratory facilities should have sufficient bench-top area for processing samples;
storage space for media, glassware, and portable equipment; floor space for stationary
equipment (incubators, water baths, refrigerators, etc.); and associated areas for cleaning
glassware and sterilizing materials. The laboratory must have the equipment and supplies
needed to perform the approved methods for which certification has been requested.

pH Meter: Accuracy and scale graduations must be within ±0.1 units. pH buffer
aliquots should be used only once. Electrodes should be maintained according to the
manufacturer's recommendations. pH meters should be standardized before each use period
with pH 7.0 and either pH 4.0 or 10.0 standard buffers, whichever range covers the desired
pH of the media or reagent. The date and buffers used should be recorded in a log book.
Commercial buffer solution containers should be dated upon receipt, and when opened.
Buffers should be discarded before the expiration date.

Conductivity Meter: should be suitable for checking laboratory reagent-grade water

and readable in appropriate M units (micromhos or microsiemens per centimeter). Use
an instrument capable of measuring conductivity with an error not more than 1% or 1
micromho per centimeter. Cell constant should be determined monthly using a method

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indicated in "Conductivity," in Standard Methods. Monthly calibration checks using an

appropriate certified and traceable low-level standard may be substituted for determining
cell constant. If an in-line unit cannot be calibrated, it should not be used to check
reagent-grade water.

Balance (top loader or pan): Balances should have readability of 0.1 g , Balances
should be calibrated monthly using ASTM type 1, 2, or 3 weights (minimum of three
traceable weights which bracket laboratory weighing needs). Non-reference weights should
be calibrated every six months with reference weights. Service contracts or internal
maintenance protocols and maintenance records should be available. Maintenance should be
conducted annually at a minimum. A record of the most recent calibration should be
available for inspection. Correction values should be on file and used. A reference weight
should be re-certified if it is damaged or corroded.

Temperature Monitoring Device: Glass, or electronic thermometers must be graduated

in 0.5 oC or less. Calibrations of glass and electronic thermometers should be checked
annually, calibration factor should be indicated on the thermometer. Also, the laboratory
should record date thermometer was calibrated and calibration factor in a QC record book. If
a thermometer differs by more than 1 oC from reference thermometer, it should be discarded.
Reference thermometers should be recalibrated every three years. Continuous recording
devices that are used to monitor incubator temperature should be recalibrated at least
annually. A reference thermometer that meets specifications should be used for calibration.

Incubator Unit: must have an internal temperature monitoring device and maintain
a temperature of 35 ±0.5 oC, and if used, 44.5 ±0.2 oC. For non-portable incubators,
thermometers should be placed on the top and bottom shelves of the use area with the
thermometer bulb immersed in liquid (except for electronic thermometers). Calibration-
corrected temperature should be recorded for days in use at least twice per day with readings
separated by at least 4 hours.

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Autoclave: is a device to sterilize equipment and supplies by subjecting them to high

pressure saturated steam at 121 oC or more, typically for 15-20 minutes depending on the
size of the load and the contents. It should have an internal heat source, a temperature gauge
with a sensor on the exhaust, a pressure gauge, and an operational safety valve. It should
maintain a sterilization temperature during the sterilizing cycle and complete an entire cycle
within 45 minutes when a 12-15 minute sterilization period is used. The autoclave should
depressurize slowly enough to ensure that media will not boil over and bubbles will not form
in inverted tubes. The date, contents, sterilization time and temperature, total time for each
cycle, and analyst's initials should be recorded each time the autoclave is used. A copy of the
service contract or internal maintenance protocol and maintenance records should be kept.

Maintenance should be conducted annually at a minimum. A record of most recent

service performed should be available for inspection. A maximum-temperature-registering
thermometer or continuous recording device should be used during each autoclave cycle to
ensure that proper temperature was reached, and the temperature recorded. Overcrowding
should be avoided. Automatic timing mechanisms should be checked quarterly with
a stopwatch or other accurate timepiece or time signal. Autoclave door seals should be clean
and free of contaminates. Also, autoclave drain screens should be cleaned frequently.

Hot Air Oven: should maintain a stable sterilization temperature of 170-180 oC for at
least two hours. Only dry items should be sterilized with a hot air oven. Overcrowding
should be avoided. Oven thermometer should be graduated in 10oC or less. Date, contents,
sterilization time and temperature of each cycle, and analyst's initials should be recorded.

Refrigerator: should maintain a temperature of 1-5 oC. Thermometers should be

graduated in at least 1oC and the thermometer bulb immersed in liquid. The temperature
should be recorded for days in use at least once per day.

Membrane Filtration Equipment (if MF procedure is used) MF units must be stainless

steel, glass, or autoclavable plastic, not scratched or corroded, and must not leak. If
graduation marks on clear glass or plastic funnels are used to measure sample volume, their

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accuracy should be checked with a standard graduated cylinder, and a record of this
calibration check retained. Membrane filters must be approved by the manufacturer.
Approval is based on data from tests for toxicity, recovery, retention, and absence of growth-
promoting substances. Filters must be cellulose ester, white, gridmarked, 47 mm diameter,
and 0.45 m pore size, or alternate pore sizes if the manufacturer provides performance data
equal to or better than the 0.45 m pore size. Membrane filters must be purchased
presterilized or autoclaved for 10 minutes at 121 oC before use. The lot number for
membrane filters and the date received should be recorded.

Glassware and Plasticware: Glassware must be borosilicate glass or other corrosion-

resistant glass and free of chips and cracks. Markings on graduated cylinders and pipets must
be legible. Plastic items must be clear and non-toxic to microorganisms. Graduated cylinders
for measurement of sample volumes must have a accurate of 2.5% or less. In graduated
cylinders, precalibrated containers that have clearly marked volumes of 2.5% tolerance may
be used. The calibration of each new lot of precalibrated containers should be validated by
selecting at least one container at random and checking calibration using a previously
verified graduated cylinder.

To sterilize and maintain sterility of glass pipets, stainless steel or aluminum canisters
should be used, or individual pipets should be wrapped in char-resistant paper or aluminum
foil. Pipets must have legible markings. Opened packs of disposable sterile pipets should be
resealed between use periods. Pipets delivering volumes of 10 mL or less must be accurate
within a 2.5%. Calibrated micropipettes may be used if tips are sterile. Micropipettes should
be calibrated annually and replaced if the accurate is greater than 2.5%.

Glassware Washing: A glassware inhibitory residue test should be performed before

initial use of a washing compound and whenever a different formulation of washing
compound, or washing procedure, is used. In addition, batches of dry glassware should be
spot-checked occasionally for pH reaction, especially if glassware is soaked in alkali or acid.
These tests will ensure that glassware is at a neutral pH and is free of toxic residue.

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Laboratory glassware should be washed with a detergent designed for laboratory use.
Distilled or deionized water should be used for final rinse.

Ultraviolet lamp (if used) The unit should be disconnected monthly and the lamps
cleaned by wiping with a soft cloth moistened with ethanol. If a UV lamp (254 nm) is used
for sanitization, lamp should be tested quarterly with a UV light meter or agar spread plate.
The lamp should be replaced if it emits less than 70% of its initial output or if an agar spread
plate containing 200 to 250 microorganisms, exposed to the UV light for two minutes, does
not show a count reduction of 99%. Other methods may be used to test a lamp if data
demonstrate that they are as effective as the two suggested methods.

Reagent-Grade Water : Only satisfactorily tested water from stills or deionization units
may be used to prepare media, reagents, and dilution/rinse water for performing
bacteriological analyses. The quality of the reagent water should be tested and should meet
the following criteria:

Parameter Limits Frequency

Conductivity <2 micromhos/cm at 25°C Monthly

Pb, Cd, Cr, Cu, Ni, Zn Not greater than 0.05 mg/L per contaminant. Annually
Total Chlorine Residual1 < 0.1 mg/L Monthly
Heterotrophic Plate Count2 < 500/mL Monthly
Bacteriological Quality of Reagent Water3 Ratio of growth rate 0.8:3.0 Annually

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Sampling, Sample Handling and Preparation

Sample: A portion of material selected to represent a larger body of material.

Sample handling: This refers to the manipulation to which samples are exposed during the
sampling process, from the selection from the original material through to the disposal of all
samples and test portions.

Subsample: This refers to a portion of the sample obtained by selection or division; an

individual unit of the lot taken as part of the sample or; the final unit of multistage sampling.

Laboratory sample: Primary material delivered to the laboratory.

Test Sample: The sample prepared from the laboratory sample.

Sample preparation: This describes the procedures followed to select the test portion from
the sample (or subsample) and includes: in-laboratory processing; mixing; reducing; coning
& quartering; riffling; and milling & grinding.

Test portion: This refers to the actual material weighed or measured for the analysis.

Once received into the laboratory, laboratory sample(s) may require further treatment
such as subdivision and or milling and grinding prior to analysis. Unless otherwise specified
the test portion taken for analysis must be representative of the laboratory sample. To ensure
that the test portion is homogeneous it may be necessary to reduce the particle size by
grinding or milling. If the laboratory sample is large it may be necessary to subdivide it prior
to grinding or milling.

Care should be taken to ensure that segregation does not occur during subdivision. In
some cases it will be necessary to crush or coarsely grind the sample prior to subdivision
into test samples. The sample maybe subdivided by a variety of mechanisms, including
coning and quartering, riffling, or by means of a rotating sample divider or a centrifugal
divider. The particle size reduction step may be performed either manually (mortar & pestle)
or mechanically using crushers or mills.

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Laboratory Measurement

The most common types of measurements are gravimetric (weighing), electrochemical

(using meters with electrodes) and optical (including visual). Instrumental methods are
becoming increasingly popular, and instrumentation is getting "smarter" and easier to use
with the inclusion of microprocessors.

In the simplest case, a sample may just be placed in an instrument and a result read
directly on a display. More often some physical separation technique or chemical procedure
is needed before a measurement is made, in order to remove interferences and transform the
analyte - target of analysis - into a form which can be detected by the instrument.

For toxic metals and organic compounds of industrial origin, measurements are now
routinely made in the part per billion (microgram per liter) range or even lower. At such low
levels, sensitive equipment and careful technique are clearly necessary for accurate results.
Avoiding contamination of the sample and using methods which prevent interferences from
other substances in the water are crucial requirements for successful analyses.

Strategy of Laboratory Measurement

All analytical work should be adequately planned. Such a plan may, in its most basic
form, be simply a notebook entry. More detailed plans will be appropriate for larger, more
complicated tasks. For work carried out under GLP, there is a specific requirement that the
work be performed to documented study plans. Plans will typically indicate the starting and
intended finishing point of the particular task together with the strategy for achieving the
desired aims. Where, during the course of the work, it is appropriate to change the strategy,
the plan should be amended accordingly.

Non-routine analysis can be considered as either tasks, but which are carried out
infrequently, where reliable methodology is already established or tasks where every sample
requires a different approach and methodology has to be established at the time.

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For such non-routine analysis some of the costs can be reduced by use of generic
methods, i.e. methods which are very broadly applicable. In other instances, subcontracting
the work to a laboratory that specializes in the particular type of work would be the most
cost-effective solution. However, where work is subcontracted, appropriate QA procedures
must be in place. In simple terms, a measurement can conveniently be described in terms of
an isolation stage and a measurement stage. Rarely can an analyte be measured without first
separating it from the sample matrix.

The value of such methods for non-routine analysis is that where a new analyte/matrix
combination is encountered, it is frequently possible to incorporate it within an existing
generic method with appropriate additional validation, measurement uncertainty calculations
and documentation. Thus the additional costs incurred are minimized in comparison to the
development of a whole new method.

The method should define the checks which will need to be carried out for the different
analyte or sample type in order to check that the analysis is valid. Sufficient information will
need to be recorded in order that the work can be repeated in precisely the same manner at
a later date. Where a particular analysis subsequently becomes routine, a specific method
may be validated and documented.

It is possible to accredit non-routine analysis and most accreditation bodies will have
a policy for assessing such methods and describing them in the laboratory's accreditation
scope or schedule. The onus will be on the laboratory to demonstrate to the assessors that in
using these techniques, it is meeting all of the criteria of the relevant quality standard. In
particular, the experience, expertise and training of the staff involved will be a major factor
in determining whether or not such analyses can be accredited.

It is the laboratory's responsibility to use methods which appropriate for the required
application, laboratory may use its own judgment, it may select a method in consultation
with customer, or method may be specified in regulation or by customer. Quality standards
often favor the use of standard or collaboratively tested methods wherever possible.

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Whilst this may be desirable in situations where a method is to be widely used, or

defined in regulation, sometimes a laboratory may have a more suitable method of its own.
The most important considerations are that the method should be suitable for the purpose
intended, be adequately validated and documented and provide results that are traceable to
stated references at an appropriate level of uncertainty.

The validation of a standard or collaboratively tested methods should not be taken for
granted, no matter how impeccable the method's pedigree, the laboratory should satisfy itself
that the degree of validation of a particular method is adequate for the required purpose, and
that the laboratory is itself able to verify any stated performance criteria.

Methods developed in-house must be adequately validated, documented and authorized

before use. Where they are available, matrix matched reference materials should be used to
determine any bias, or where this is not possible, results should be compared with other
technique(s), preferably based on different principles of measurement.

Developments in methodology and techniques will require methods to be changed from

time to time and therefore method documentation must be subject to adequate document
control. Each copy of the method should show issue number/date, issuing authority, and
copy number. It must be possible to determine from records which is the most up-to-date
version of each method is authorized for use.

Obsolete methods should be withdrawn but must be retained for archive purposes and
clearly labeled as obsolete. The difference in performance between revised and obsolete
methods should be established so that it is possible to compare new and old data.

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Laboratory Instrumental Analysis

The costs of chemical measurement reflect the costs associated with the various stages
of method development, validation, instrumentation, consumables, ongoing maintenance,
staff input, calibration, quality control, etc. Many of these costs are independent of the
number of samples subsequently analyzed using that method. Thus where a single method
can be used for a large throughput of samples, unit analytical costs will be comparatively
low. Where a method has to be specially developed for just a few samples, the unit
analytical costs can be very high. Thus, the purpose of the isolation stage is to simplify the
matrix in which the analyte is finally measured.

Often the isolation procedure may vary very little for a wide variety of analytes in
range of sample matrices. A good example of a generic isolation procedure is the digestion
technique to isolate trace metals in foods. Similarly, once analytes have been isolated from
the sample matrix and are presented in a comparatively clean environment, such as solvent,
it may be possible to have a single generic method to cover the measurement of a wide
variety of analytes. For example, gas chromatography, or UV-visible spectrophotometry,
documentation of such generic methods should be designed so that it can easily
accommodate the small changes which relate to the extraction, clean-up or measurement of
different analytes, for example by the use of tables. The sort of parameters which might be
varied are sample size, amount and type of extraction solvents, extraction conditions,
chromatographic columns or separation conditions, or spectrometer wavelength settings.

Measurement of the recovery of gravimetrically added spike analyte, measurement of

blanks and the study of interferences and matrix effects can also be used to check for bias or
imperfect recovery. Estimation of uncertainty must form part of this validation process and
in addition to covering the above factors, should address issues such as sample homogeneity
and sample stability. Documentation of methods shall include validation data, limitations of
applicability, procedures for quality control, calibration and document control. A laboratory
documenting methods may find it convenient to adopt a common format, such as ISO 78,
which provides a useful model.

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Spectroscopy Analysis

 Electromagnetic Spectrum

Frequency : The number of oscillations of an electromagnetic wave per second

Wavelength : The distance between any two consecutive maxima or minima of an electromagnetic wave

When an atom or molecule absorbs energy, electrons are promoted from their ground
state to an excited state. In a molecule, the atoms can rotate and vibrate with respect to each
other. These vibrations and rotations also have discrete energy levels, which can be
considered as being packed on top of each electronic level.

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Beer-Lambert law

A : Absorption a : Molar absorptivity (absorptivity constant)

C : Concentration b : Path length (width of the cell)

Absorbance depends on the total quantity of the absorbing compound in the light
path through the cuvette. If we plot absorbance against concentration, we get a straight
line passing through the origin (0,0) We will Note that the Law is not obeyed at high
concentrations. This deviation from the Law is not dealt with here. The linear relationship
between concentration and absorbance is both simple and straightforward, which is
why we prefer to express the Beer-Lambert law using absorbance as a measure of the
absorption rather than %T.

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Usually a working curve is devised. The absorbance's of a series of three to five standard
solutions are measured and plotted on graph paper against the concentrations of these
standards. This is known as a Beer's Law plot. The absorbance of an unknown concentration
is then measured and its concentration is determined directly from the plot. This is an
extremely common application in Chemistry.

Many compounds absorb ultraviolet (UV) or visible (Vis.) light. The diagram below
shows a beam of monochromatic radiation of radiant power I0, directed at a sample solution.
Absorption takes place and the beam of radiation leaving the sample has radiant power I.

Deviations from Beer’s Law

Beer’s Law is usually followed at low concentrations of analyte for homogeneous

samples. Absorbance is directly proportional to concentration for most absorbing substances
when the concentration is less than about 0.01 M. Deviations from linearity are common at
high concentrations of analyte. There are several possible reasons for deviation from
linearity at high concentrations.

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At low concentrations in a solution, the analyte would be considered the solute. As the
solute concentration increases, the analyte molecules may begin to interact with each other,
through intermolecular attractive forces such as hydrogen bonding and other van der Waals
forces. Such interactions may change the absorptivity of the analyte, again resulting in a
nonlinear response as concentration increases.

A Spectrophotometer is an instrument that measures transmission of light through

a substance. When light is absorbed by a sample, radiant power of light beam decreases.
Radiant power, P, refers to the energy per second per unit area of the beam, light passes
through a monochromator that selects one wavelength. Light of this wavelength, with
radiant power P0 , strikes a sample of length b . Radiant power of the beam emerging from
the other side of the sample is P. Some of the light may be absorbed by the sample, P ≤ P0

UV-Vis. Molecular Spectroscopy

The energy states associated with molecules, like those of atoms, are also quantized.
There are very powerful spectroscopic methods for studying transitions between permitted
states in molecules using radiation from the radiowave region to the UV region. These
methods provide qualitative and quantitative information about molecules, including
detailed information about molecular structure.

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Unlike atoms, the energy states in molecules have rotational and vibrational sublevels, so
when a molecule is excited electronically, there is often a simultaneous change in the
vibrational and rotational energies. The total energy change is the sum of the electronic,
rotational, and vibrational energy changes.

Because molecules possess many possible rotational and vibrational states, absorption of
UV or visible radiation by a large population of molecules, each in a slightly different state
of rotation and vibration, results in absorption over a wide range of wavelengths, called an
absorption band.

The UV/VIS absorption spectra of molecules usually have a few broad absorption bands
and are usually very simple in comparison with IR spectra. Molecular absorption and
emission spectroscopy is used for qualitative identification of chemical species, especially
for inorganic and organometallic molecules with metal atoms at their centers.

This technique used to be one of the major methods for structural determination of
organic molecules, but has been replaced by the more powerful and now commonly
available techniques of NMR, IR spectroscopy, and MS.

UV/VIS absorption spectroscopy is most often used for quantitative analysis of the
molecular composition of samples. Molecular fluorescence spectroscopy is an extremely
high sensitivity method, with the ability to detect single molecules!

Calibration & Analysis

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Atomic Absorption Spectrometry (AAS)

The technique known as atomic absorption spectroscopy is of particular analytical

importance for the determination of metals due to its sensitivity and potential for selectivity
by virtue of the narrow atomic absorption lines. A schematic representation of the
spectrophotometer is shown in Fig. To take advantage of characteristic selectivity, a special
radiation source must be provided to produce extremely monochromatic radiation with a
linewidth less than the absorption bandwidth of the atomic sample. In most cases the same
element being analyzed is also used in the source lamp to provide appropriate emission
line spectra by stimulation with a plasma discharge.

Common sources are hollow cathode lamps, electrodeless discharge lamps, and gaseous
discharge lamps. The source is often modulated and coupled to a lock-in amplifier in order
to determine the relative absorbance of the atomic sample as compared with sample
emission at the same wavelength.

Other methods of background correction involve monitoring of a non absorbed radiation

by the use of distinct spectral lines, continuous sources, or the Zeeman effect (separation of
degenerate energy states of an atom by application of a powerful magnetic field; provides
closely spaced energy levels which are sensitive to polarized light).

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The sample itself is usually produced by volatilization of solutions in a high-temperature

flame or solids and in a graphite furnace. Flame methods generally provide relative errors of
approximately 1–2%, whereas the equivalent furnace methods provide only 5–10%, but
sensitivities up to 1000 times greater than those observed for flames. Chemical interferences
commonly originate from the atmosphere supporting the atomic population and from other
sample matrix components.

The formation of oxides in flames causes the reduction of the atomic population and can
be controlled by the employment of appropriate fuel–oxidant ratios and by sampling
appropriate portions of the flame. This problem is avoided in the furnace by the use of
a continuous flowing inert gas atmosphere. Poor volatilization and atomization often occur
when an analyte binds with anions in the sample matrix. This is overcome by the use of high
concentrations of cationic releasing agents, which preferentially couple with the interferent,
or by the use of protective agents such as chelating ligands, which form stable but volatile
species with the analyte of interest.

Spectral interferences can also occur, though direct overlap of interferent and analyte
atomic absorption bands is rare. These interferences include molecular band absorption such
as that experienced from the formation of combustion products, which can often be
eliminated by the use of higher temperatures, and ionization of the atomic population due to
excess temperatures.

Since many of the chemical processes occurring in certain localized areas of atomic
atmosphere are approximately in equilibrium, such ionization can be suppressed by addition
of a radiation buffer, which selectively ionizes in contrast to analyte of interest and therefore
increases the probability of ion–electron recombination to form the required atomic
population. Atomic spectroscopy is a principal tool for measuring metallic elements at parts
per million and lower (parts per billion) in industrial and environmental laboratories. This
allow each instrument to turn out hundreds of analyses per day.

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In atomic spectroscopy, a liquid sample is aspirated (sucked) though a plastic tube into
a flame is measured either by its absorption or emission of radiation. For atomic absorption
spectroscopy, radiation of the correct frequency is shined through the flam and transmitted
radiation is measured. For atomic emission spectroscopy, no lamp is required.

Radiation is emitted by hot atoms whose electrons have been promoted to exited state in
the flame. For both monochromator is used to select the wavelength of radiation that will be
viewed by the detector. Because the lines of wavelength are so sharp, there is usually little
overlap between the spectra of different elements in the same sample. This allow to some
instruments to measure over 60 elements in sample simultaneously.

Atomic Absorption Spectroscopy, measure absorption energy which need to remove

electron from ground state to exited state (ionization energy) of the atoms which directly
proportional with concentration of the molecules (atoms of the elements), where is atom
absorb light from lamp (Hollow Cathode Lamp) and unabsorbed light reaches the detector.

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Inductively Coupled Plasma (ICP)

Inductively Coupled Plasma (ICP) is an analytical technique used for the detection of
trace metals in environmental samples. The primary goal of ICP is to get elements to emit
characteristic wavelength specific light which can then be measured. The technology for the
ICP method was first employed in the early 1960's with the intention of improving upon
crystal growing techniques. Since then, ICP has been refined and used in conjunction with
other procedures for quantitative analysis. Following is a cursory look at the driving forces
behind this analytical tool, its use in series with other analytical tools, and environmental
applications of ICP.

The definition of plasma is an electrically neutral (Inert to some extent) gas made up of
positive ions and free electrons. Plasmas have sufficiently high energy to atomize, ionize,
and excite virtually all elements in the periodic table, which are intentionally introduced into
it for the purpose of elemental chemical analysis. Although there are many types of plasmas
(direct current, microwave induced, etc.) the inductively coupled plasma (ICP) has
demonstrated the most useful properties as an ion source for analytical mass spectrometry.

Gases such as argon, helium, nitrogen, and air have been used to sustain plasmas useful
for analytical purposes; however, the inert gases offer some advantages, because of their
desirable ionization properties and their avail- ability in relatively pure form. Impurities in
the plasma support gas can result in spectral interferences, leading to inaccurate quantitative
measurements. Inert gases, specifically argon, also have the advantageous property of
minimal chemical reactivity with various analyte species, which can also result in
undesirable analytical results.

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Workings of an ICP

ICP hardware is designed to generate plasma, which is a gas in which atoms are present
in an ionized state. The basic set up of an ICP consists of three concentric tubes, most often
made of silica. These tubes, termed outer loop, intermediate loop, and inner loop,
collectively make up the torch of the ICP. The torch is situated within a water-cooled coil of
a radio frequency (r.f.) generator. As flowing gases are introduced into the torch, the r.f field
is activated and the gas in the coil region is made electrically conductive. This sequence of
events forms the plasma.

Plasma: A hot, ionized gas containing an abundance of ions and electrons.

Plasma Sources: Plasma consists of a hot, partially ionized gas, containing an abundant
concentration of cations and electrons that make the plasma a conductor. The plasmas used
in atomic emission are formed by ionizing a flowing stream of argon, producing argon ions
and electrons. The high temperatures in a plasma result from resistive heating that develops
due to the movement of the electrons and argon ions.

Because plasmas operate at much higher temperatures than flames, they provide better
atomization and more highly populated excited states. Besides neutral atoms, the higher
temperatures of plasma also produce ions of the analyte.

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Plasma formation: Inductively coupled plasmas are formed by coupling energy produced by
a RF generator to the plasma support gas with an electromagnetic field. The field is
produced by applying an R F power (typically 700-1500 W) to an antenna (load coil)
constructed from 3-mm-diameter copper tubing wrapped in a two- or three-turn 3-cm-
diameter coil, positioned around the quartz torch assembly designed to configure and
confine the plasma. An alternating current field is created that oscillates at the frequency of
the tuned RF generator.

The plasma is initiated by the addition of a few “seed” electrons, generated from the
spark of a Tesla coil or a piezoelectric starter, to the flowing support gas in the vicinity of
the load coil. After the plasma is initiated it is sustained by a process known as inductive
coupling. As these seed electrons are accelerated by the electromagnetic RF field, collisions
with neutral gas atoms create the ionized medium of the plasma.

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These collisions produce additional electrons. This cascading effect creates and sustains
the plasma. Once the gas is ionized, it is self-sustaining as long as RF power is applied to the
load coil. The ICP has the appearance of an intensely bright fireball-shaped discharge.

The resulting collisions with the abundant unionized gas give rise to resistive heating,
providing temperatures as high as 10,000 K at the base of the plasma, and between 6000 and
8000 K at a height of 15–20 mm above the coil, where emission is usually measured. At
these high temperatures the outer quartz tube must be thermally isolated from the plasma.

The formation of the plasma is dependent upon an adequate magnetic field strength and
the pattern of the gas streams follows a particular rotationally symmetrically pattern. The
plasma is maintained by inductive heating of the flowing gases. The induction of a magnetic
field generates a high frequency annular electric current within the conductor. The
conductor, in turn, is heated as the result of its ohmic resistance.

This energy is sufficient to accelerate ionized particles into many collisions which cause
further ionization and emission of significant background radiation from the argon gas. The
plasma is ignited by seeding with electrons generated by an electrical discharge. After the
onset, the plasma becomes a self-propagating and -sustaining process. The tangentially
introduced argon gas (Fig.) spins the plasma into a torroidal shape at the point where the
sample is introduced. The sample is injected into the center of the plasma where excitation is
more efficient. As shown in Fig. , the plasma may be divided into observation zones where
atomic or ionic species are more abundant.

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Chromatography Analysis

Separation is a familiar word, and it is unlikely that any confusion will arise from its use
in reference to chemical analysis. Nevertheless, there is some merit in considering a precise,
general definition such as that suggested by Rony:

"Separation is the hypothetical condition where there is complete isolation, by separate

macroscopic regions, for each of the chemical components which comprise a mixture. In other
words, the goal of any separation process is to isolate the chemical components, in their pure
forms, into separate vessels, such as glass vials or polyethylene bottles."

The adjective hypothetical is used for two reasons. In the first place, it is theoretically
impossible to accomplish the complete separation of the components of a mixture. Consider,
for example, the process of analyte transfer in a liquid-liquid extraction. If a single
extraction removes most of the analyte from phase 1 into phase 2, say 90%, each successive
step will also remove 90% of the analyte that remained after the previous step. Thus 10% of
the analyte from the previous step remains in the first phase and subsequent steps can
remove only a fraction (0.9) of it.

Clearly, all of the analyte cannot be removed; of course, when the fraction removed
approaches 1, say 0.9999, we consider that virtually all of it has been removed. The second
reason for using the term hypothetical is that the separated components often are not actually
isolated into vessels but rather are detected and their presence recorded (on chart paper or in
a computer data file).

Theory of Chromatography

Most separation methods employ two phases. In chromatography, they are called the
mobile phase and the stationary phase. In liquid-liquid extraction, they are called the
extractant and the raffinate. The extractant in a multistage liquid-liquid extraction has
a function similar to the mobile phase in liquid chromatography, and comparisons of these
two techniques will help in understanding both of them. In distillation, the second phase
(a vapor) is formed from the first phase (a liquid) as the latter is heated.

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This process differs from extraction and chromatography where the second phase is
added. Obviously, the principles of distillation are different from those for chromatography.
However, as has been noted, much of the development of GC was carried out by chemists
who were accustomed to making their separations by distillation, so they labeled the
chromatographic process with distillation terms such as theoretical plutes.

A sample that requires analysis is often a mixture of many components in a complex

matrix. For samples containing unknown compounds, components must be separated from
each other so that each individual component can be identified by other analytical methods.
Separation properties of components in a mixture are constant under constant conditions,
and therefore once determined they can be used to identify and quantify each of components.
Such procedures are typical in chromatographic and electrophoretic analytical separations.

A mixture can be separated using the differences in physical or chemical properties of

the individual components. As an example, dumping spaghetti and water in a colander
separates the two components because the liquid water can run through the colander but the
solid spaghetti cannot. Some water will stick to the spaghetti and some spaghetti may go
down the drain because the colander is not 100% efficient.

An analogous example is the filtering of a solid precipitate to separate it from a solution.

These separations are based on states of matter of two components; other physical properties
that are useful for separations are density and size. Some useful chemical properties by
which compounds can be separated are solubility, boiling point, and vapor pressure.

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In chromatography, one phase is held immobile or stationary and the other one (the
mobile phase) is passed over it, as noted above. Strictly speaking, in current practice, many
stationary phases nominally listed as liquids are really chemically bonded to (or chemically
polymerized and cross-linked to) a solid support [as in bonded-phase (BP) HPLC] or to the
column wall (as in capillary GC). The IUPAC definition of chromatography is:

“Chromatography is a physical method of separation in which the components to be

separated are distributed between two phases, one of which is stationary (stationary phase)
while the other (the mobile phase) moves in a definite direction. Elution chromatography is
a procedure in which the mobile phase is continually passed through or along the
chromatographic bed and the sample is fed into the system in a definite slug."

Mobile phase In HPLC, TLC, and CZE the mobile phase is a liquid that moves through
past a stationary phase and causes separation. In GC separations, the mobile phase is a gas
(often called the carrier gas).

Stationary phase The retentive component(s) of the packing material. In adsorption

chromatography the packing material itself is the stationary phase, whereas in partition
chromatography the adsorbed liquid phase or bonded phase is the stationary phase.

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At any given time, a particular analyte molecule is either in the mobile phase, moving
along at its velocity, or in the stationary phase and not moving at all in the downstream
direction. The sorption-desorption process occurs many times as the molecule moves
through the bed, and the time required to do so depends mainly on the proportion of time it
is sorbed and held immobile.

A separation is effected if the various components emerge from the bed at different
times, which are called retention times. The status of the separation is shown at five
different times-five snapshots of the separation. In the first one, the mixture of analytes

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A and B is introduced to the bed in as narrow a zone as possible. The mobile phase, flowing
from left to right, carries them along the bed. Since all the molecules of a particular analyte
do not encounter the exact same local environment in the stationary and mobile phases, the
peak for that analyte will have a finite width in the chromatogram.

Note that the width of the peaks increases with the length of time they remain in the bed.
Because analyte A has a greater affinity for the mobile phase, it spends more time in the
mobile phase and travels faster and elutes before analyte B. Thus A and B become separated.
Another, less popular form of chromatography is controlled by displacement. The sample is
pushed through the system by displacing it from the stationary bed with other sample
components and a strong mobile phase.

The chromatographic process we have defined is also known as zonal or hatch

chromatography because the sample is applied to the system all at once in one narrow zone.
By contrast, the sample can be applied continuously during a run; this process is called
frontal analysis. One application to immune affinity chromatography has been published
recently, but it will not be discussed further here because of its limited use.

The mode of interaction between the sample components and the two phases can be
classified into two types, although many separation processes are combinations of both. If
the sample is attracted to the surfaces of the phases, commonly to the surface of a solid
stationary phase, the process is called adsorption. Alternatively, if the sample diffuses into
the interior of the stationary phase-for example, into the bulk of a stationary liquid
chromatographers call the process partition. Actually, absorption seems to be a better name
for this process because we can then speak of sorption as the general process and add the
prefixes ah or ad when we want to be more specific. For this reason, the terms absorption
and adsorption will be used in this monograph even though partition is the term
recommended by the IUPAC.

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Gas Chromatography (GC)

The publication in 1952 of James and Martin's study' on gas chromatography (GC).
Since that time, GC has become the premier technique for the separation and analysis of
volatile compounds and gas chromatographs have been the most widely used analytical
instrument in world, although HPLC is becoming more widely used.

Clearly, GC is a major analytical method and it is complemented by other major form

of Chromatography, HPLC, which is capable of handling non volatiles not suited to GC.
The currently accepted status between them is that GC can be used up to 350°C
corresponding to an upper molecular weight limit of 600 D," and HPLC is used for higher
molecular weight compounds.

Before GC became popular in the late 1950s, the only way to separate volatile materials
was by distillation, which separates materials based on differences in vapor pressure or
boiling point. GC is similar, but its separations also depend on the nature of the stationary
phase, which gives it much more versatility than distillation.

Imagine the pleasure and surprise of separations chemists who could now separate
materials with close boiling points, such as benzene and cyclo-hexane (The boiling points of
benzene and cyclo-hexane are nearly same, 80.1 and 81.4 oC). And it was easy, fast, and not
too expensive; in addition, they did not have to worry about azeotropes.

Gas chromatography is a chromatographic technique that can be used to separate volatile

organic compounds. A gas chromatograph consists of a flowing mobile phase, an injection
port, a separation column containing the stationary phase, and a detector. The organic

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compounds are separated due to differences in their partitioning behavior between the
mobile gas phase and the stationary phase in the column.

The earliest columns were packed with solids or with solid supports coated with liquids.
In accordance with our naming convention, these two types of chromatography are called
gas-solid chromatography (GSC) and gas-liquid chromatography (GLC).

In 1957 Golay published his ideas for using columns that were not packed but were open
tubes.’ These tubes had to have small inside diameters; they were capillary columns, but the
name open tubular (OT) columns is more descriptive and preferred when comparing them to
packed columns. In OT columns, the SP can be coated on, or bonded to, the inside wall, and
these columns are called wall-coated OT columns (WCOT).

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In GC, mobile phase, usually helium is inert and does not participate in the chemistry of
the chromatographic process but only serves to carry the sample through the column. Hence,
the theory of GC is concerned only with the interactions between the SP and the analytes.

Starting with that base, the following discussion shows how GC theory has developed in
an attempt to explain in more elaborate terms the effectiveness of the SP in effecting
separations like the one just illustrated, benzene and cyclohexane.

The essential parts of a gas chromatograph as shown in Figure are: carrier gas, flow or
pressure regulator, injection port/splitter, column, and detector. Usually there are three
separate heated zones, for the injector, the column, and detector.

Connections between these heated zones must also be kept hot enough to prevent
condensation of analytes in them. Chromatographs designed for OT columns have an
injection port that allows for sample splitting and a provision for some additional “makeup”
gas for the detector, as shown.

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Mobile phases are generally inert gases such as helium, argon, or nitrogen. The most
popular carrier gases are nitrogen, helium, and hydrogen. They must be very pure, and they
are chosen for their inertness since, as we have seen, their only purpose is to carry the
analyte vapors through the column.

Helium is the most popular because of its higher efficiency at faster flow rates, the
optimum velocity for Helium is around 20-30 cm/s, but little efficiency is lost at higher
velocities, so most chromatographers run their OT columns around twice optimum velocity.
Since helium is expensive and in limited supply in some parts of the world, hydrogen is
increasing in popularity, but its use requires additional safety precautions to prevent
explosions. However, these advantages are not as impressive for programmed temperature
GC as they are for isothermal GC, so helium remains the gas of choice for most laboratories.
Sometimes the choice of carrier is dictated by the detector.

The normal sequence of events in a GC injection is as follows. We will assume in this

explanation that some analytes are dissolved in a (liquid) solvent although much of this
process also holds for gas GC injections too. A small amount of liquid (micro liters) is
injected through a silicon rubber septum (using a special micro liter syringe) into the hot
(usually +200o C) GC injector that is lined with an inert glass tube.

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The injector is kept hot by a relatively large, metal heater block that is thermostatically
controlled. The sample is immediately vaporized and a pressurized, inert, carrier gas-which
is continually flowing from a gas regulator through the injector and into the GC column-
sweeps the gaseous sample, solvent, analyte and all, onto the column.

In gas chromatography two basic types of sampling system are used, those suitable for
packed columns and those designed for open tubular columns. In addition, different sample
injectors are necessary that will be appropriate for alternative column configurations.

It must be stressed, however, that irrespective of the design of the associated equipment,
the precision and accuracy of a GC analysis will only be as good as that provided by the
sample injector. The sample injector is a very critical part of the chromatographic equipment
and needs to be well designed and well maintained.

There are two types of columns in common use in GC and they are the packed column
and the open tubular column. The former are usually 2 to 4 mm I.D. and 1 to 4 meters long
and, packed with a suitable adsorbent, are mostly used for gas analysis. As a result of the
simpler injection procedure and the more precise sampling method, the packed column tends
to give greater quantitative accuracy and precision. However, despite its problems with
sample injection, the open tubular column is the most popular column system in general use.
The length of open tubular columns range from about 10 m to 100 m and can have internal
diameters from 100 µm to 500 µm. Stationary phase is coated on the internal wall of the
column as a film 0.2 µm to 1 µm thick.

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After the components of a mixture are separated using gas chromatography, they must be
detected as they exit the GC column. The links listed below provide the details of some
specific GC detectors. The thermal-conductivity (TCD) and flame-ionization (FID) detectors
are the two most common detectors on commercial gas chromatographs.

The requirements of a GC detector depends on the separation application. For example,

one analysis might require a detector that is selective for chlorine-containing molecules;
another analysis might require a detector that is non-destructive so that the analytes can be
recovered for further spectroscopic analysis, FID is usually required for OT chromatographs
because of its greater sensitivity. Both are classified and compared in Table.

Quantitative Analysis

There are three important stages in a GC analysis,

- The preparation of the sample.
- The development of the separation and the production of the chromatogram
- The processing of the data and the presentation of the results.

Each stage is equally important and if not carried out correctly the results will be neither
precise nor accurate. Sample preparation can be very simple involving no more that diluting
a known weight of sample with mobile phase or be much more complex including an
extraction procedure followed by derivatization and then dilution.

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Liquid Chromatography (HPLC, IC)

Liquid chromatography (LC) is an analytical chromatographic technique that is useful

for separating ions or molecules that are dissolved in a solvent. If the sample solution is in
contact with a second solid or liquid phase, the different solutes will interact with the other
phase to differing degrees due to differences in adsorption, ion-exchange, partitioning, or
size. These differences allow the mixture components to be separated from each other by
using these differences to determine the transit time of the solutes through a column.

Simple liquid chromatography consists of a column with a fritted bottom that holds
a stationary phase in equilibrium with a solvent. Typical stationary phases (and their
interactions with the solutes) are: solids (adsorption), ionic groups on a resin (ion-exchange),
liquids on an inert solid support (partitioning), and porous inert particles (size-exclusion).
The mixture to be separated is loaded onto the top of the column followed by more
solvent. The different components in the sample mixture pass through the column at
different rates due to differences in their portioning behavior between the mobile liquid
phase and the stationary phase. The compounds are separated by collecting aliquots of the
column effluent as a function of time.

Schematic of a simple liquid chromatographic separation

Conventional LC is most commonly used in preparative scale work to purify and isolate
some components of a mixture. It is used in ultra-trace separations where small disposable
columns are used once and then discarded. Analytical separations of solutions for detection
or quantification typically use more sophisticated high-performance liquid chromatography
instruments. HPLC instruments use a pump to force the mobile phase through and provide

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higher resolution and faster analysis time. Today, liquid chromatography, in its various
forms, has become one of the most powerful tools in analytical chemistry.

Liquid chromatography can be performed using planar Techniques or column techniques

Column liquid chromatography is the most powerful and has the highest capacity for
sample. In all cases, the sample first must be dissolved in a liquid that is then transported
either onto, or into, the chromatographic device.

High-Performance Liquid Chromatography (HPLC)

It is a form of liquid chromatography to separate compounds that dissolved in solution.

HPLC instruments consist of a reservoir of mobile phase, a pump, an injector, a separation
column, and a detector. Compounds are separated by injecting a plug of the sample mixture
onto the column. The different components in the mixture pass through the column at
different rates due to differences in their partitioning behavior between the mobile liquid
phase and the stationary phase.

In the beginning, pumps only had a pressure capability of (500 psi) (35 bars). This was
called high pressure liquid chromatography (HPLC). The early 1970s saw a tremendous leap
in technology. These new HPLC instruments could develop up to 6,000 psi (400 bars) of
pressure, and incorporated improved injectors, detectors, and columns. HPLC really began
to take hold in the mid-to late-1970s. With continued advances in performance during this
time (smaller particles, even higher pressure), the acronym remained the same, but the name
was changed to high-performance liquid chromatography (HPLC).

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High-performance liquid chromatography (HPLC) is now one of the most powerful tools
in analytical chemistry. It has the ability to separate, identify, and quantities the compounds
that are present in any sample that can be dissolved in a liquid. Today, compounds in trace
concentrations as low as parts per trillion (ppt) may easily be identified. HPLC can be, and
has been, applied to just about any sample, such as pharmaceuticals, food, environmental
matrices, forensic samples, and industrial chemicals.

High-performance liquid chromatography, often called simply by its abbreviation, HPLC

constitutes a general purpose analytical technique derived from the most ancient form of
preparative liquid chromatography. The modern day technique is greatly enhanced in terms
of selectivity, resolution, through miniaturization and the use of very elaborate stationary
phases. These phases comprise spherical micro-particles with diameters of 2–5µm, or
porous monolithic material that leads to a significant pressure drop on the column. A large
pressure needs to be exerted upon the mobile phase to obtain a continuous flow.

In spotting this particularity, the letter P of the abbreviation corresponded for a long time
to the word pressure. The forced migration of a liquid phase in continuous contact with
a stationary phase is encountered in several chromatographic techniques. One of the aspects
particular to HPLC is that of the partition mechanisms between analyte, mobile phase and
stationary phase. They are based on coefficients of adsorption or partition.

Compare GC with HPLC. The typical capillary GC column has an internal diameter
around 0.25 mm (or 250 µm). A typical polymer stationary phase coating on the inner wall
of this capillary is 0.25 µm (or 250 nm). The high diffusion rate of analytes in the gas phase
permits rapid near-equilibration over such distances. Diffusion in a liquid is much slower. If
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we compensate by reducing the dimensions of a capillary LC system sufficiently to attain

the desired near equilibration condition, they will be very small indeed, with a bore
measured in a few microns. To retain a phase ratio similar to GC, the stationary coating must
shrink to a thickness of several nanometers (nm).

This is in the size range of single molecules. An open-tubular LC column with such
dimensions would have a very minimal sample capacity before it overloaded, and it would
be very difficult to build a detector that would work on such a small scale. Larger volume
detectors would introduce severe extra-column band broadening or require extensive
makeup flow which would further dilute the already miniscule concentrations of analyte
eluting from such a column. Capillary HPLC is possible when samples are limited to very
small amounts, but it is nowhere near as common as capillary GC.

The way to achieve HPLC is to return to packed columns, but to implement them with
support particle and stationary phase coating dimensions much smaller than those of packed
column GC. Typically one employs spherical silica particles of uniform diameters
(monodisperse) in the range of 2–10 µm. The pore spaces between the tightly packed
spheres will be of similar dimension. Unlike the much larger support particles in packed
column GC, these LC particles often have a smaller scale secondary internal porosity of
channels permeating the particle into which analytes can diffuse. Here are some points of
contrast between HPLC and packed or capillary GC stationary phases:

- Each LC phase molecule is bonded to its solid support surface, but is less often
cross-linked. The HPLC phase is so thin that it is not a fully randomized fluid, like a
GC polymer coating.

- Because of smaller particle size and internal porosity of LC packings, area covered by
molecular monolayer stationary “phase” is vastly greater than that of thick polymer
film stationary phase in GC columns of similar volume. This restores analyte capacity
of these columns to a level compatible with typical chromatographic detector designs.

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- The HPLC columns must operate at pressures, (500–6000 vs. 10–50 psi), orders of
magnitude higher than GC columns. Mobile phase must be pumped instead of coming
from a pressurized cylinder through a reducing valve. Columns are commonly
fabricated from thick-walled stainless steel, with stainless steel mesh packing
restraining frits, and use stainless steel or high impact plastic nut and ferrule fittings.

- Dissolved gases in mobile phase may come out of solution and form bubbles as the
pressure changes from entrance to the exit of the column. Those will block and channel
flow, degrading resolution or even blocking the column completely. Even if bubbles
redissolve, resultant large cavity in packing may introduce extra-column band
broadening. Mobile phase liquids must be degassed prior to use, by filtering under
vacuum or by sparging with a flow of fine bubbles of poorly soluble helium gas.

- The small interparticle pore size of HPLC columns requires stable, uniform, spherical
particles to avoid their packing together in a fashion which will block uniform flow
through these tiny passages. Mobile phase solvents must be filtered to remove micron-
size particles which could plug up these interstitial pores and block or channel mobile
phase flow.

- As the composition of the liquid mobile phase is varied, it can interact to cause
alterations in the alignment of the stationary phase molecules, and thereby affect their
partition behavior with some analytes. This dependence of stationary phase behavior
upon mobile phase composition is not found in GC, and it needs more complexity to
prediction of HPLC separation behavior.

- As the instrument cycles the column through very large pressure changes as the pumps
turn flow on and off, the packed bed may move or settle, yet again introducing the
dread void and its extra-column band broadening.

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Three of the most common nonpolar organic substituents employed in stationary phases
for HPLC with aqueous/polar mobile phases are:

The larger the substituent group, the more strongly and longer will it retain the nonpolar
analyte, so retention will vary inversely to the order listed here.
Three examples of common polar organic substituents (incorporating functional groups
to confer the desired polarity) for normal phase HPLC with less-polar mobile phases are:

Here it is the functional groups which dominate retention. Amino and Diol phases will
retain compounds with pronounced hydrogen bonding potential more strongly, while Cyano
phase interacts most strongly with analytes whose polar interactions result from strong
dipole moments. Complex structures may interact in a combination of these mechanisms, so
relative retention is less easy to predict than with the reversed phase columns.

The degree of interaction between the mobile phase and the stationary phase whether
normal or reversed, affects the retention time of the analytes. In principle, the polarity of the
stationary phase can lead to the following situations:

o If the stationary phase is polar, technique said to be normal phase chromatography

o If the stationary phase is non-polar, technique is called reversed phase chromatography

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Ion Chromatography

Ion chromatography is a form of liquid chromatography that uses ion-exchange resins to

separate atomic or molecular ions based on their interaction with the resin. Its greatest utility
is for analysis of anions for which there are no other rapid analytical methods. It is also
commonly used for cations and biochemical species such as amino acids and proteins. Most
ion-exchange separations are done with pumps and metal columns. Simple LC columns are
used to separate one ion from others in ultra-trace analytical applications.

Columns of ion-exchange resins have been used for many years to separate certain
cations and anions from one another. Cations are separated on a cation exchange resin
column, and anions are separated on a column containing an anion exchange resin. The most
used types are as follows:

For example, Na+ and K+ can be separated on a cation-exchange resin (Catex) column
with a dilute solution of a strong acid (H+) as eluent (mobile phase). Introduction of sample
causes Na+ and K+ to be taken up in a band (zone) near top of column by ion exchange.

Continued elution of the column with an acidic eluent H+ introduces competition of H+,
Na+ and K+ for the exchange sites (-SO3-) causing the Na+ and K+ zones to move down the

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column. K+ is more strongly retained than Na+; thus the Na+ zone moves down the column
faster than the K+ zone. As originally conceived and carried out for many years, fractions of
effluent were collected from the end of the column and analyzed for Na+ and K+. Then a plot
was made of concentration vs. fraction number to construct a chromatogram, all of the Na+
would be in a single fraction of several milliliters and all of the K + could be recovered in a
second fraction of a certain volume.

Thus, under predetermined conditions, each ion to be separated could be collected in a

single fraction and then analyzed by spectroscopy, titration, etc., to determine the amount of
each sample ion. The situation regarding ion-exchange chromatography changed suddenly
and drastically in 1975 when a landmark paper was published by Small, Stevens and
Bauman. Smaller and more efficient resin columns were used. But, more importantly, a
system was introduced using a conductivity detector that made it possible to automatically
detect and record the chromatogram of a separation.

A new name was also introduced: ion chromatography. This name was originally applied
to a patented system that used a conductivity detector in conjunction with a second ion-
exchange column called a suppressor. However, the name “ion chromatography” is now
applied to any modern, efficient separation that uses automatic detection.

In suppressed ion chromatography, anions separated on a separator column that contains

a low-capacity anion-exchange resin. A dilute solution of a base, such as sodium carbonate,
sodium bicarbonate or sodium hydroxide is used as the eluent. Immediately following the
anion-exchange “separator” column, a cation-exchange unit (called the suppressor) is used
to convert the eluent to molecular carbonic acid, which has a very low conductivity.

Also, counter ions of sample anions are converted from sodium to hydrogen. The eluate
from the suppressor unit then passes into a conductivity detector. If the sample ion pair is
ionized to a reasonable extent, the sample anion (and the H+ counter ion) is detected by
conductivity. An example of a state-of-the-art separation in the 1970s is shown in next Fig.

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In the earlier instruments, the suppressor unit was a cation-exchange column of high
capacity that had to be regenerated periodically. Newer suppressors contain ion exchange
membranes that can be regenerated continuously by flowing a solution of sulfuric acid over
the outer membrane surface or by electrically generated acid.

For non-suppressed ion chromatography to be successful, the ion exchanger used in the
separation column must have a low exchange capacity and a very dilute eluent must be used.
In the separation of anions, the resin must have an exchange capacity between about 0.005
mequiv/g and 0.10 mequiv/g.

Typical eluents are 1.0 x l0-4 M solutions of sodium or potassium salts of benzoic acid.
hydroxybenzoic acid, or phthnlic acid. These eluents are sufficiently dilute that the
background conductivity is quite low. Most sample anions have a higher equivalent
conductance than that of the eluent anion and can therefore be detected even when present in
concentrations in the low parts per million range.

For separation of cations, a cation exchange column of low capacity used in conjunction
with either a conductivity detector or another type of detector. With a conductivity detector,
a dilute solution of nitric acid is typically used for separation of monovalent cations, and
a solution of an ethylene-di-ammonium salt is used for separation of divalent cations.
Because both of these eluents are more highly conducting than the sample cations, sample
peaks are negative relative to background (decreasing conductivity).

IC became an almost overnight sensation. It now became possible to separate mixtures

such as F-, CI-, Br-, NO3- and S042- in minutes at low ppm concentrations. Analytical
problems that many never knew existed were described in an avalanche of publications.

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Electro-chemical Analysis

pH measurement

pH meter (probe and meter) For accurate measurements and use in dilute solutions,
electrochemical measurement (a "pH meter") is required. To read the H + ion concentration.
Laboratory pH meters are often made with a glass electrode consisting of a silver wire
coated with silver chloride immersed in dilute hydrochloric acid. The electrode solution is
separated from the solution to be measured by a thin glass membrane.

The potential which develops across that glass membrane can be shown to be
proportional to the hydrogen ion concentrations on the two surfaces. In the measurement
instrument, a cell is made with the other electrode commonly being a mercury-mercury
chloride electrode. The cell potential is then linearly proportional to pH and the meter can
then be calibrated to read directly in pH.

We can measure pH by pH meter by used probe (electrode) and meter by this steps:

- Calibrate the probe and meter according to the manufacturer’s directions. Use of two
buffers (pH 7 and 10) for calibration is recommended.
- Sample water can be collected in any glass or plastic container. Collect enough
sample water so that you can submerge the tip of the probe. Rinse the probe with
sample water before placing it in the sample.

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- Place the probe in the sample and wait for the meter to equilibrate. If the meter needs
to be manually adjusted to correct for temperature – you’ll know it does if it has an
extra temperature knob – adjust it to the temperature of the sample before allowing it
to equilibrate. The meter will have come to equilibrium when the signal becomes
steady. If it is taking a long time to equilibrate, you may try gently stirring the probe.
However, do not agitate the sample since this may cause changes in the pH.

- Read the pH directly from the meter according to the manufacturer’s directions.

Accuracy and scale graduations must be within ±0.1 units. pH buffer aliquots should be
used only once. Electrodes should be maintained according to the manufacturer's
recommendations. pH meters should be standardized before each use period with pH 7.0 and
either pH 4.0 or 10.0 standard buffers, whichever range covers the desired pH of the media
or reagent. The date and buffers used should be recorded in a log book. Commercial buffer
solution containers should be dated upon receipt, and when opened. Buffers should be
discarded before the expiration date.

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Conductivity Measurement

Conductivity or specific conductance is the measure of the water's ability to conduct an

electric current. Conductivity depends upon the number of ions or charged particles (such as
salt) in the water. The ease or difficulty of the flow of electrical current through liquids
makes it possible to divide them into two broad categories: electrolytes and non electrolytes.

Electricity passes easily through water that is high in electrolytes or ions, and poorly
through low electrolyte such as pure water or many organic solvents such as alcohol or oil.
The opposition to flow of electricity is called resistance and it is measured in units called
ohms. Substances with low resistance and high conductivity pass electricity easily.

Pure water, such as distilled water, will have a very low specific conductance, and sea
water will have a high specific conductance. Rainwater often dissolves airborne gasses and
airborne dust while it is in the air, and thus often has a higher specific conductance than
distilled water. Specific conductance is an important water-quality measurement because it
gives a good idea of the amount of dissolved material in the water.

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Electrical conductivity is a measure of water’s ability to conduct electricity, and

therefore a measure of the water’s ionic activity and content. The higher the concentration
of ionic (dissolved) constituents, the higher the conductivity. Conductivity of the same
water changes substantially as its temperature changes. This can have a confounding effect
on attempts to compare this feature across different waters, or seasonal changes in this
parameter for a particular body of water.

The use of specific conductance [SC; units of micro Siemens per centimeter (µS·cm-1)
or mile Siemens per centimeter (mS·cm-1), 1 Siemens = 0.9534 ohm], the conductivity
normalized to temperature of 25 ºC, eliminates this complication and allows valuable
comparisons to be made.

By definition, specific conductivity is the reciprocal of the specific resistance of

a solution measured between two electrodes 1 cm2 in area and 1 cm apart. Conductivity is
thus measured by placing two electrodes (with opposite electrical charge) in the water.

For a known electrical current, the voltage drop across the electrodes reveals the water’s
resistance. Since the resistance of aqueous solution changes with temperature (resistance
drops with increasing temperature), the resistance is corrected to the resistance of the
solution at 25 ºC

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A conductivity meter is used to measure ability of water sample to conduct electricity.

The specific conductance is measured by passing a current between two electrodes (one
centimeter apart) that are placed into a sample of water. The unit of measurement for
conductivity is expressed in either microSiemens (uS/cm) or micromhos (umho/cm) which is
the reciprocal of the unit of resistance, the ohm.

The prefix "micro" means that it is measured in millionths of a mho. MicroSiemens and
micromhos are equivalent units. Distilled water has a range of conductivity from 0.5 to 2
µmhos/cm. Drinking water is generally between 50 to 1500 µmhos/cm.

Meters should be suitable for checking laboratory reagent-grade water and readable in
appropriate M units (micromhos or microsiemens per centimeter). Use an instrument
capable of measuring conductivity with an error not more than 1% or 1 micromho per
centimeter. Cell constant should be determined monthly using a method indicated in
"Conductivity," in Standard Methods.

Monthly calibration checks using an appropriate certified and traceable low-level

standard may be substituted for determining cell constant. If an in-line unit cannot be
calibrated, it should not be used to check reagent-grade water.

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DO Measurement

D.O. can be measured by a fairly tricky wet chemical procedure known as the Winkler
titration. The D.O. is first trapped, or "fixed", as an orange-colored oxide of manganese. This
is then dissolved with sulfuric acid in the presence of iodide ion, which is converted to
iodine by the oxidized manganese. The iodine is titrated using standard sodium thiosulfate.
The original dissolved oxygen concentration is calculated from the volume of thiosulfate
solution needed.

Measurements of D.O. made more conveniently with electrochemical instrumentation.

"D.O. meters" are subject to less interference than the Winkler titration. They are portable
and can be calibrated directly by using the oxygen in the air. DO meter and electrode work
in similar fashion to other electronic meters but unlike the others, this meter must be
continually "on" to remain polarized.

To be "on" the electrode must be continuously attached to the meter and the meter must
be either plugged into an AC outlet or if battery operated, the battery must be good. If the
battery fails, or the meter is unplugged, the DO electrode must be re polarized for an hour
before being used to measure a sample.

DO meters must be calibrated following the manufacturer's instructions. Since oxygen is

a gas, it is influenced by the barometric pressure and temperature. The manufacturer
provides a table that can be used to determine the saturated DO level at different elevations
and temperatures. Meters are commonly calibrated against a saturated air solution. It is
a good idea to periodically validate the DO calibration using the Winkler Titration Method.

A functioning membrane is essential to good DO measurement. The membrane allows

oxygen to permeate to the electrode where it creates a mill-volts current directly proportional
to the DO concentration. One of the major advantages of the electrode method is that it can
be used continuously.

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The DO electrode can be submerged in the stream to different depths or in an aeration

basin and the DO monitored continuously. However, the membrane does not last indefinitely
and must be changed frequently. DO electrode, the membrane at the end of the probe
requires periodic replacement.

Maintaining will help the lab analyst predict when failure is likely to occur. Replacing
the membrane should only take a couple of minutes. Follow the manufacturer’s instructions
and be sure to use the manufacturer’s recommended filling solution.

The filling solution is not the same as the KCl used for the pH meter. The electrode
should be disconnected from the meter when the membrane is replaced. If the membrane has
been replaced properly there should be no air bubbles beneath the membrane.

The DO should be measured at a representative point. Remember dissolved oxygen is

a gas and is affected by turbulence and temperature. Measuring a DO sample at a point of
high turbulence will not be representative. Likewise, measuring DO in shallow or quiet areas
of a river will be different than in deeper and faster moving areas. A sampling plan will help
define what information is needed and where the most appropriate location will be.

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Instrumentals Calibration

Calibration is a set of operations that establish, under specified conditions, the

relationship between values of quantities indicated by a measuring instrument or measuring
system, or values represented by a material measure, and the corresponding values realized
by standards The usual way to perform calibration is to subject known amounts of the
quantity (e.g. using a measurement standard or reference material) to the measurement
process and monitor the measurement response. The overall programmed for calibration in
the chemical laboratory shall be designed to ensure that all measurements that have
a significant effect on test or calibration results are traceable to a measurement standard,
preferably a national or international measurement standard such as a reference material.

Where appropriate and where feasible, certified reference materials should be used.
Where formally designated measurement standards are not available, a material with
suitable properties and stability should be selected or prepared by the laboratory and used as
a laboratory measurement standard. The required properties of this material should be
characterized by repeat testing, preferably by more than one laboratory and using a variety
of validated methods

Analytical tests may be sub-divided into general classes depending on the type
of calibration required: Some analytical tests depend critically on the measurement of
physical properties, such as weight measurement in gravimetry and volume measurement in
titrimetry. Since these measurements have a significant effect on the results of the test,
a suitable calibration programmed for these quantities is essential. In addition, the
calibration of measuring devices used to establish the purity or amount concentration of the
chemical standards, need to be considered. Where a test is used to measure an empirical
property of a sample, such as flashpoint, equipment is often defined in a national or
international standard method and traceable reference materials should be used for
calibration purposes where available. New or newly acquired equipment must be checked by
laboratory before use to ensure conformity with specified design, performance and
dimension requirements.

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Instruments such as chromatographs and spectrometers, which require calibration as

part of their normal operation, should be calibrated using reference materials of known
composition (probably solutions of pure chemicals). In some cases, calibration of the whole
analytical process can be carried out by comparing the measurement output from a sample
with the output produced by a suitable reference material that has been subjected to the same
full analytical process as the sample.

For example calibration of a gas chromatography method may be carried out using
a series of measurement standards which are synthetic solutions of the analyte of interest at
various concentrations. Such calibration does not take into account factors such as
contamination or losses that occur during the sample preparation and extraction.

It is therefore essential during the method validation process to explore the potential
problems of contamination and losses by taking matrix reference materials or spiked
samples through the whole measurement process, and design the day to- day calibration
procedure and quality control checks accordingly. Individual calibration programmes shall
be established depending on the specific requirements of the analysis.

Also, it may be necessary to check instrument calibration after any shutdown, whether
deliberate or otherwise, and following service or other substantial maintenance. The level
and frequency of calibration should be based on previous experience and should be at least
that recommended by the manufacturer.

The calibration of volumetric glassware normally relates to a particular solvent at

a particular temperature. The calibration is rarely valid when the glassware is used with
other solvents because of different densities, wetting characteristics, surface tension etc. This
is particularly pertinent for volumetric glassware calibrated to deliver a certain volume.

Other volumetric equipment may be affected when using solvents with high rates of
thermal expansion. In such situations the glassware should be recalibrated using the relevant
solvent, at the correct temperature. Alternatively, for the highest accuracy, measurements
can often be made by mass rather than by volume.

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Method of calibration

Calibration is the process of establishing the relationship between the signal we

measure (such as absorbance) and known concentrations of analyte. Once this relationship is
established, it is possible to calculate the concentration of the analyte in an unknown sample
by measuring its signal. The calibration methods discussed subsequently are applicable to
most of the analytical instrumental methods, not just spectroscopic measurements.

In order to use Beer’s Law to determine the concentration of analyte in an unknown, it

is necessary to establish the relationship between absorbance at a given wavelength and the
concentration of the analyte. Solutions containing known concentrations of analyte are
called standard solutions or more simply, standards.

For some types of analyses, the standards may be in the form of solids or gases.
Standards must be prepared accurately from high purity materials so that the concentration
of analyte is known as accurately as possible.

A series of standards covering an appropriate concentration range is prepared. The

standards should include one solution with no added analyte; the concentration of analyte in
this standard is zero. This solution is called the reagent blank and accounts for absorbance
due to impurities in the solvent and other reagents used to prepare the samples.

It also accounts for the instrumental baseline. The absorbance of the reagent blank and
each standard is measured. The absorbance of the reagent blank is subtracted from the
absorbances of the other standards before any calculations are performed.

The absorbances from which the blank absorbance has been subtracted are called
“corrected absorbances”. A plot is made of corrected absorbance on the y-axis vs. the
known concentration of the standard on the x-axis. Such a plot used to be constructed
manually on graph paper; now, plots are generated by computer software.

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For example calibration curve which show the relationship between the absorbance of
n-hexadecane, CH3(CH2)14CH3, a hydrocarbon found in petroleum, at 3.41 µm in the IR
region and the concentration of solutions of n-hexadecane in tetrachloroethylene, C 2Cl4. This
measurement of the absorbance of solutions of n-hexadecane at 3.41 µm is a method used
for determining petroleum contamination in water, soil, and other environmental samples,
because most hydrocarbons absorb at this wavelength.

It is an official method developed by the US EPA and relies on Beer’s Law to permit
the measurement of petroleum hydrocarbons in unknown samples. It is used to measure
environmental contamination from oil spills, illegal dumping of oil, and leaking
underground oil storage tanks.

Performing a linear regression on the data in Table provides us with the exact Beer’s
Law relationship for this method: A = 0.0250x - 0.001, where x is the concentration of
n-hexadecane (in mg/100 mL). From the equation for the calibration curve, the
concentration can be determined for any measured absorbance.

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Quality Control and Quality Assurance

A laboratory may apply QA to all or part of its operations. Where a laboratory claims
compliance against, or certification or accreditation to, a particular standard, it is important
to be clear to what this compliance, certification or accreditation applies. The formal
statement of the activities which have been certified against ISO 9001 or accredited against
ISO 17025 is known as the "scope". ISO 9000 and GLP require only a brief description of
the activities covered, but with ISO/IEC 17025, a detailed description of the specific work
covered by the accreditation is usually required.

Quality management is aided by a clear statement of activities, which ideally should

define the range of work covered, but without restricting the laboratory's operation. Different
quality standards have different rules, but for ISO/IEC 17025, the scope may typically be
defined in terms of: the range of products, materials or sample types tested or analyzed; the
measurements (or types of measurements) carried out; the specification or method,
equipment, technique; concentration, range and measurement uncertainty as appropriate.

Definition of scope in specific terms is clearly most easily applied to laboratories

carrying out routine testing to established procedures. Where non-routine testing is carried
out, a more flexible approach to scope is desirable. The scope must, however, be as specific
as is feasible and the QA system maintained by the laboratory must ensure that the quality of
the results is under control.

A laboratory wishing to change its scope, either by adding additional tests or changing
the methodology of existing tests will require the approval of the accreditation body, who
will have specified policy for such situations. Typically, it is possible to grant simple
changes by examination of documentation. For more complex changes, particularly where
new techniques are involved, additional assessment may be required. There are a number of
important terms used in quality management and conformity assessment whose meaning
may vary according to the context in which they are used. It is important to understand the
distinction between the various terms.

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Quality: Degree to which a set of inherent characteristics fulfils requirements

Accreditation: ‘Procedure by which an authoritative body gives formal recognition that

a body or person is competent to carry out specific tasks’. In the context of a laboratory
making measurements, accreditation is a formal recognition that a laboratory is competent to
carry out specific calibrations or tests or specific types of calibrations or tests. The
mechanism under which accreditation is granted is described in requirements document is
ISO/IEC 17025. Accreditation is also used in the context of ISO 9000 based activities to
describe the process whereby a national organization formally recognizes certification
bodies as competent to assess and certify organizations as being compliant with the ISO
9000 series of standards (“quality management systems”).

Certification: ‘Procedure by which a third party gives written assurance that a product,
process or service conforms to specified requirements’ (ISO Guide 2:1996). Certification,
(sometimes known as registration) primarily differs from accreditation in that technical
competence is not specifically addressed.

Quality Assurance (QA): QA describes the overall measures that a laboratory uses to ensure
the quality of its operations. Typically this might include:
 A quality system
 Suitable laboratory environment
 Educated, trained and skilled staff
 Equipment suitably maintained and calibrated
 Quality control procedures
 Documented and validated methods
 Traceability and measurement uncertainty
 Checking and reporting procedures
 Preventative and corrective actions
 Internal audit and review procedures
 Complaints procedures
 Requirements for reagents, calibrates, measurement standards materials
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Quality Control (QC): ‘The operational techniques and activities that are used to fulfill
requirements for quality'. Quality control procedures relate to ensuring the quality of specific
samples or batches of samples and include:

 Analysis of reference materials/measurement standards

 Analysis of blind samples
 Use of quality control samples & control charts
 Analysis of blanks
 Analysis of spiked samples
 Analysis in duplicate
 Proficiency Testing

Audit and Review: In practice quality audits take two forms. An audit carried out by an
independent external body as part of the accreditation process is more usually known as an
assessment. “Quality audits” carried out within the laboratory, are sometimes subdivided
into audit, often called ‘internal audit’, (which checks that the quality procedures are in
place, and fully implemented) and review (which checks to ensure that the quality system is
effective and achieves objectives. The review is carried out by senior management with
responsibility for the quality policy and work of the laboratory.

Standard: This word has a number of different meanings in the English language. In the past
it has been used routinely to refer firstly to written standards, i.e. widely adopted procedures,
specifications, technical recommendations, etc., and secondly, to chemical or physical
standards used for calibration purposes. In this guide, to minimize confusion, standard is
used only in the sense of written standards.

The term measurement standard is used to describe chemical or physical standards,

used for calibration or validation purposes, such as: chemicals of established purity and their
corresponding solutions of known concentration; UV filters; weights, etc. Reference
materials are one (important) category of measurement standards.

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 Chemical laboratory; Operations, Equipment,
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Reference Material (RM): ‘Material or substance one or more of whose property values are
sufficiently homogeneous and well established to be used for the calibration of an apparatus,
the assessment of a measurement method, or for assigning values to materials.

Certified Reference Material (CRM): ‘Reference material, accompanied by a certificate, one

or more of whose property values certified by a procedure, which establishes its traceability
to an accurate realization of the units in which the property values are expressed, and for
which each certified value is accompanied by an uncertainty at a stated level of confidence’

Traceability: Property of the result of a measurement or the value of a standard whereby it

can be related to stated references, usually national or international standards, through an
unbroken chain of comparisons all has stated uncertainties.

Measurement Uncertainty: a parameter associated with the result of a measurement that

characterizes the dispersion of the values that could reasonably be attributed to the measure.

Laboratory Audit and Review

An important aspect of quality management is the periodic re-examination of the

quality system by the laboratory's own management. In general, all aspects of the quality
system should be examined at least once a year.

The system should be examined in two ways. Firstly, it should be examined to ensure
that it is sufficiently well documented to enable adequate and consistent implementation, and
that staff are actually following the system described.

This examination is commonly known as auditing (as opposed to the external auditing
or assessment carried out by accreditation or certification bodies). Secondly, the system
should be examined to see whether it meets the requirements of the laboratory, its customers
and, if appropriate, the quality management standard.

Over a period of time the needs of the laboratory and its customers will change and the
quality system should evolve to continue to fulfill its purpose. This second type of
examination is commonly known as review and should be carried out at least annually. It is

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 Chemical laboratory; Operations, Equipment,
Instruments, Quality & Safety

carried out by the laboratory management and draws on information from a number of
sources, including results from internal audits, external assessments, proficiency testing
scheme participation, internal quality control studies, market trends, customer complaints
and compliments, etc.

The programmed of audits and review is normally co-ordinated by the laboratory

quality manager, who is responsible for ensuring that auditors have the correct training,
guidance and authority necessary for their work. Audits are normally carried out by
laboratory staffs who work outside of the area they are examining. This is of course not
always possible where staff numbers are small. Audits may be carried out in two basic
ways. In the horizontal audit, the auditor will examine in detail single aspects of the quality
system, for example calibration or reports. In the vertical audit the auditor will select
a sample and follow its progress from receipt to disposal, examining all aspects of the
quality system relating to its testing.

114 Chemist/ Essam Eldin Metwally Ahmed www.sites.google.com/view/essamdin