Contents

1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating and drying
apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
LABORATORY APPARATUS
 What are the lab apparatus you have used?

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3
LABORATORY APPARATUS

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4
LABORATORY APPARATUS

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5
 DESSICATORS

Hygroscopic
samples (absorb
moisture)

Drying Cabinet

[Link]
dhs
 Desiccant

The most common desiccant is silica, an otherwise inert,

nontoxic, water-insoluble white solid. Tens of thousands of
tons are produced annually for this purpose.

Other common desiccants include activated charcoal,

calcium sulfate, calcium chloride, and molecular sieves
(typically, zeolites).
WEIGHING BOTTLES

•Weighing bottle are

used for drying

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samples.
•Hygroscopic samples
are weighed by
differences, keeping the
bottle capped except
when removing the
sample

7
 Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
TOPIC 2
Apparatus & Techniques
ANALYTICAL BALANCE
 An analytical balance is an instrument that is
used to obtain 4 to 5 digits to the right of decimal
point.

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 All analytical balances require a “wind screen” or
“cabinet” in order to realize the required
precision of the measurements.
 Measure mass to a very high degree of precision
(0.1 or 0.01 mg)

10
TYPES OF BALANCES

Single pan
analytical

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mechanical balance

Auxillary balance
Balances
(Top pan balance)

Electronic
analytical balance
11
ANALYTICAL BALANCE
 A weighing boat or dish is used for direct
weighing of samples.

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11
PLACEMENT OF ANALYTICAL BALANCE

 Explain what is wrong of this situation?

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13
PLACEMENT OF ANALYTICAL BALANCE

 The balance should not be placed near an open

window or directly in front of the air-condition air
vent. This will cause draft.

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14
PLACEMENT OF ANALYTICAL BALANCE

 Explain what is wrong with this situation

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 The balance should have a stable support, usually a
concrete bench.
15
PLACEMENT OF ANALYTICAL BALANCE

 Explain what is wrong with this situation

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 The balance should not be placed where there is
direct sunlight.
15
PLACEMENT OF ANALYTICAL BALANCE

 Explain what is wrong with this situation

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 The room temperature is too high. The room
should be air-conditioned.
17
PLACEMENT OF ANALYTICAL BALANCE

 Stability
 Temperature and evaporation

 Far from drafts (movement of air)

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CARE & USES
 Always handle the analytical balance with great
care. Never drop it!
 Keep clean.

18
 Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
TOPIC 2
Apparatus & Techniques
GENERAL RULES FOR WEIGHING
 The balance should be warmed up for at least half an hour before
use.
 Before turning on, ensure all the doors are closed and the pan is
not touching the draft ring.
Never handle objects to be weighed with fingers. Use tongs or

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
finger pads (gloves) to prevent uptake of moisture by dried
objects.
 Centre the substance to be weighed in the middle of the pan.
 Weigh at room temperature.
 Never place chemicals directly on the pan, but weigh them in a
vessel (dish, boat, weighing bottle, small beaker)
 Always brush spilled chemicals off immediately with a soft
brush.
 Always close the balance case door before making the weighing.
Air currents will cause the balance to be unsteady.
20
USE OF THE ANALYTICAL BALANCE
 Press the TARE on the balance to zero the
display.
 Place a sheet of quantitative filter paper on the

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pan of the balance.
 Use a clean, dry spatula to carefully measure the
required quantity of solute calculated.
 Read the display weight after the display is
stable, indicated by the no-motion symbol
switches on or off.
 Record the weight of the solute for reference.

21
 WEIGHING OF SOLIDS

Direct weighing Weighing by difference

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 Solid chemical
 A weighing materials are usually
dish/bottle/boat is used. weighed and dried in a
weighing bottle.
 The dish is weighed
 Replicate weighing are
empty and then with the most conveniently
sample. carried out by weighing
 Direct weighing is
the difference.
satisfactory only if the  Also if the sample is
hygroscopic, weighing 21
sample is non- by difference with the
hygroscopic. bottle capped must be
employed.
TECHNIQUE OF WEIGHING BY DIFFERENCE

 The sample in the weighing bottle is weighed,

and then a portion is removed and quantitatively
transferred to a vessel.

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 Then the weighing bottle and the sample is re-
weighed, and from the difference in weight, the
weight of sample is calculated.
 The next sample is transferred and the weight is
repeated to get its weight by difference, and so
on.

22
 WEIGHING OF LIQUID

Direct weighing Weighing by difference

 By pipetting out an
The liquid is aliquot from the
transferred to a weighing bottle, the

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inside of the pipette
weighing vessel must be rinsed
(e,g, a weighing several times after
bottle) which is transferring.
capped to prevent  Care should be taken
not to lose any sample
evaporation from the tip of the
during the pipette during
weighing, and transferring. 23

then weighed.
 ERROR IN WEIGHING

 Weighing in the vacuum is the most accurate.

 The weighing are made on a balance will, of course, give
the weight in air. When an object displaces its volume in
air, it will buoyed up by the weight of air displaced.
(Archimedes’ principle)
 Actually in most cases, a correction is not necessary
because the error resulting from buoyancy will cancel out
in percent composition calculation.
 The same error will occur in the numerator (as the
concentration of a standard solution or weight of a
gravimetric precipitate) and in the denominator (as the
24
weighed sample)
 Of course, all weighing must be made with materials in
the same type of container (same density) to keep the
error constant.
CORRECTION FOR BUOYANCY

 A buoyancy error will affect data if the density of

the object being weighed differ significantly from
that of the standard weight.

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 This error has its origin in the difference in the
buoyant force exerted by the medium (air) on the
objects and on the weights.
 Weight of object in air can be corrected to the
weight in vacuum by:

 Wvac = Wair + Wair [ 0.0012/Do – 0.0012/Dw]

26
 Wvac = weight in vacuum/corrected mass of the
object, g
 Wair = observed weight in air, g

 Do = density of object

 Dw = density of weight

 0.0012 = density of air

EXAMPLE

 A bottle of weighed 7.6500 g empty and 9.9700 g after

filling an organic liquid with a density 0.92 gcm-3. The
balance was equipped with stainless steel weights (d

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= 8.0 gm-3). Calculate the corrected mass of the
organic liquid sample.

 Observed weight in air, Wair = (9.9700 – 7.6500) g

= 2.3200 g

W vac/corr
 2.3200 + 2.3200 [ 0.0012/0.92o –0.0012/8.0w]
27
 = 2.3227 g
Q
 A 20 mL pipet is to be calibrated. A stoppered
flask when empty weighs 29.2780 g. Water is
delivered into it from the pipet, and it now

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weighs 49.2720 g. If stainless steel weights are
used, calculate the corrected weight of water
delivered.

 Given: density of air = 0.0012 g/mL

 Density of stainless steel weights = 8.0 g/mL

28
 Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
TOPIC 2
Apparatus & Techniques
VOLUMETRIC GLASSWARE
 1. For very accurate volumetric analysis you need to calibrate the
volumetric glassware.
 2. All volumetric glass wares are allowed tolerance by

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manufacturer.
 The accuracy is usually measured in terms of
the tolerance, which is the uncertainty in a
measurement made with the glassware. Class A
volumetric glassware has a lower tolerance than Class
B; for class A, the tolerance can be as low as 0.08 ml
for a 100 ml flask or pipet.

 For example, a volumetric pipette may be labeled 25 mL, but 30

it will deliver that volume with a tolerance. A 100 mL
volumetric flask is manufactured to a tolerance of ± 0.08 mL
and since liquids and glass expand or contract as
temperature rises and falls, the tolerance applies at the
temperature indicated on the flask, usually 20 0C.
CALIBRATION OF A VOLUMETRIC FLASK
 Weigh a clean and dry volumetric flask and
record its weight.
 Fill the volumetric flask with distilled water up

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to the mark and weigh the flask again.
 Record the temperature of water.

 Calculate the mass of water in the volumetric

flask.
 Calculate the volume of water in the flask based
on the density of water at the recorded
temperature.
33
MEASURING VOLUME
 The unit of volume is liter (L)
 It is defined as one cubic decimeter (dm3)

 Milliter (ml) is one thousand of a liter

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 1 liter = 1000 ml

34
 Glassware

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Non
Volumetric
volumetric

TC
TD (To contain) TC
(To deliver) - Volumetric flask, (To contain)
pipette, graduated 33
-pipette, buret -Beaker, flask
cylinder
 Glassware

Volumetric
TC TD

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Graduated
Cylinder Pipette Burette
Volumetric
flask (For rapid (For (For titration,
measurement of transferring accurate in
(For preparation liquid volume, liquid dispensing
of standard semi-accurate between aliquots of
solution) liquid measuring containers) solutions)
vessel) 34
 Glassware

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Non Volumetric

TC
Beaker
Flask
(For transferring
liquid to another (For containing a
container) certain volume) 35
PIPETTE
 Pipette is used to transfer a
particular volume of solution.
 It permits the transfer of accurately
known volumes from one container

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to another
 It is sometimes used to deliver a
certain fraction or portion (aliquot)
of a solution

36
TYPES OF PIPETTES

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 Volumetric
 Measuring

 Mohr

 Serological
37
TWO COMMON TYPES OF PIPETTES
Volumetric or transfer pipette Measuring or graduated pipette
(bulb pipette) (TD) (clinical, Mohr or serological
pipette (TC)

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 Sizes of 100
mL to 5 mL
or less)

 The measuring
pipettes range
from total
volume of 25
mL to 0.1 mL. 38

TC or TD
 Pipettes are calibrated “to deliver” (TD) or “to contain”
(TC)
 If the pipette were calibrated TC, the small remaining
volume should be shaken or blown out to obtain the

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correct amount of material

 If the volume pipettes are calibrated to deliver (TD), a

certain small volume remaining in the tip. This should not
be shaken or blown out.

 In delivering , the pipette is held vertically and the tip is

touched on the side of the vessel to allow smooth delivery
without splashing and so that the proper volume will b3e9
left in the tip.
 BLOW OUT PIPETTES

The frosted band should

not be confused with
thicker colored rings or
colored dots, which are a
manufacturer’s code for
the maximum volume
of the pipette.

Remember, only blow-

out a serological pipette
if it has a frosted band
or two thin rings.
VOLUMETRIC PIPETTES
(TD)

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 Used for accurate measurements, since it is
designed to deliver only one volume
and is calibrated at that volume. 43

 Should be used when accuracy and

reproducibility are crucial, because these can
achieve accuracy to four significant figures.
SPECIFICATIONS ON VOLUMETRIC PIPETTE

 On a volumetric pipette, the specifications

indicate
 How much liquid will be transferred if the liquid is

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drawn up to the calibration line on the neck
 The temperature at which the calibration was made
 Whether is a TD or TC pipette

44
TD VOLUMETRIC PIPETTE
 The volumetric pipette (a bulb shaped) is used for
accurate measurements since it is designed to
deliver only one volume and is calibrated at that
volume. Volumetric pipetts are available in sizes

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of 100 mL to 0.5 mL or less.

Pipett e 5 10 25 50 100
capacity
(mL)

Tolereance 0.01 0.04 0.06 0.08 0.12 42

(mL)
 MEASURING PIPETTES

 They are straight glass or plastic tubes with one

tapering end.
 Calibrated into small divisions so that various

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amounts of liquid can be measured with the same
pipet.
 Usually used to measure any amount between
0.1 mL and 25.0 mL.
 They are not as accurate due to the fact that any
imperfection in their internal diameter will have
a greater effect on the volume delivered.
46
MEASURING PIPETTES

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SEROLOGICAL
MOHR
• The graduation
- The graduations on continues to the tip
these always end
before the tip • If a serological pipette
has a frosted band or
two thin rings around
the neck, then it is a
blow-out pipette.
47

[Link]
SPECIFICATIONS ON A MEASURING
PIPETTE

 Printed on the neck of the pipette are:

 The maximum volume of the liquid that can be
transferred

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 The size of the divisions on the pipette.
 The temperature at which calibrations were made
 If the pipette is a ‘to deliver (TD)” or ‘to contain (TC)”

48
BASIC TECHNIQUES FOR USING PIPETTE
 Clean the pipette with detergent and water.
 Rinse thoroughly, first with tap water then with Distilled
water.
 Rinse with the intended solution, twice.

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 Using a filler, fill the pipette and adjusting the meniscus to
the calibration mark. At the top of a pipette is an etched
ring. Fluid must be drawn up above a ring indicating the
volume and then released slowly until the bottom of the
meniscus is exactly at the ring.
 Hold vertically, allow water to run out with the tip of the
pipet touching the side of the receiving flask, being careful
that no fluid splashes on the neck of the receiving flask. It
is important that the neck of the flask and its stopper
remain dry throughout the experiment.
 The pipette must be held vertically. Allow to drain for 10 s 46
BURETTE
 A burette is used for the accurate delivery of
a variable amount of solution

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 Burette enable the analyst to deliver any
volume up to their maximum capacities
 Its principle use is in titration, where a
standard solution is added to the sample
solution until the end point is reached
 The conventional burette for micro titration
is marked in 0.1 ml increments from 0 to 50
ml. The volume delivered can be read to the
nearest 0.05 ml by interpolation. 47
READING BURETTE

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48
BASIC TECHNIQUES FOR USING BURETTE

 Clean the burette with detergent and water and

rinse it with distilled water.
 Check the bore and tip are clear.

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 Rinse twice with 5-10 mL portions of the
intended solution.
 Using a funnel, fill with the intended.

 Displace any air bubbles from the tip of the

burette, and adjust to near zero mark. Allow to
stand for a few minutes to check for leakage and
read the initial volume to the nearest 0.05mL.
VOLUMETRIC FLASK
 Volumetric flasks are used in the diluting of a
sample or solution to a certain volume.
 The volumetric flasks come in a variety of sizes,

ZK_CHM421_2016
ranging from 1.0 mL or more to 2.0 L.
 The flask are designed to contain an accurate
volume at the specified temperature (20 or 25
C).
 These flasks are marked with “TC” to in dicate ‘to
contain’

53
TECHNIQUES FOR USING VOLUMETRIC
FLASK

 Initially a small amount of diluent (usually

distilled water) is added to the empty flask.
 REAGENT CHEMICALS SHOULD NEVER BE

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ADDED DIRECTLY TO A DRY FLASK
SURFACE, as glass is highly absorbent to
concentrated substances.
 Then the desired chemical reagent (either solid or
liquid) is added to the flask.

54
 Then the diluent (dilution solvent) is added to fill
flask about 2/3 and flask is swirl to mix it before
diluent is further added to the neck of the flask.

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 Finally diluent is added to the meniscus carefully
in drop wise manner.
 The solution is finally thoroughly mix by
inverting the flask and swirl or shake vigorously
for 10 sec.
 Turn right side-up and repeat the invertion,
shaking or swirling for at least 10 times.
55
STEPS IN PREPARING STANDARD SOLUTION

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56
OTHER TYPES OF GLASSWARES

57
 CALIBRATION OF
GLASSWARES

1. DIRECT 2. INDIRECT
•A volume of water delivered •Volumetric glassware calibrated
by a buret or pipet, or by comparison of the mass of
contained in a volumetric water it contains or delivers at a
flask, is obtained directly particular temperature with that
from the weight of the of another vessel which had
water and its density been calibrated directly.
•The volumes are directly
related to the masses of water.
This method is convenient if
many pieces of glassware are to
be calibrated.
55
3. RELATIVE CALIBRATION
CALIBRATION OF A 50 ML VOLUMETRIC
PIPETTE

 Ensure the pipette is clean.

 Determine the mass of the empty, stoppered receiver
to the nearest milligram.

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 Transfer the 50 mL volume from pipette into a
stoppered container.
 Weigh the stoppered receiver and its contents and
calculate the mass of water delivered by difference.
 From the delivered mass of water, calculate the
volume delivered using the appropriate density data
table.
 Repeat the calibration three times and calculate the
mean volume delivered and the standard deviation. 56
CLEANING OF GLASSWARE

 Clean glassware is imperative for accurate and

precise volumetric applications.
 It is therefore necessary to thoroughly clean all

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glassware before use.

61
 Aqua regia
cleaning
solution (nitro-
hydrochloric
acid)
Warm Concentrated
Detergent Acid

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Potassium
dichromate Method for
Ultrasonic
sulphuric acid Cleaning cleaning
cleaning Glassware
solution
62
 Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
TOPIC 2
Apparatus & Techniques
DISTILLED WATER
 Distilled water is desirable as it contain no
dissolved minerals, chemicals, impurities etc.

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 The water distiller effectively removes more than
99.8% of most tap water impurities, including
crystosporidium. (Cryptosporidium is a genus
of apicomplexan protozoans that can cause
gastrointestinal illness with diarrhea in
humans.)

64
 DISTILLATION PROCESS
A. The dirty water is heated,
B. To boiling thus vapourises
C. (becomes steam), while other

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substances remain in solid state
in boiler. Steam is then directed
into a cooler,
D. Where it cools down and return
to liquid water,
E. And the end result is a water,
purified of additional substances
in it.
65
Q
 What is distilled water?
 What will be removed from distillation?

 What cannot be removed from distillation and

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why?
 What will happen to the boiler after period of
time?
 What will you do?

 What other applications of distilled water besides

using in laboratory?

66
 DEIONIZED WATER The vast majority of dissolved
impurities in modern water
supplies are ions as calcium,
The deionization sodium, chlorides etc.
process removes ions
from water via ion
exchange.
Na+, Cl-

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H+ OH-
H+ OH-
Positively charged ions (cations)
H+ negatively charged ions (anions) are OH-
exchanged for hydrogen (H+) and
Na+ hydroxyl (OH-) ions, respectively, due to
Cl-
the resin’s greater affinity for other ions.

H+, OH- 63
The ion exchange process
occurs on the binding sites
of the resin beads.
PROCESS IN DEIONIZED WATER
The vast majority of dissolved impurities in modern water
supplies are ions as calcium, sodium, chlorides etc.

The deionization process removes ions from water via

ion exchange.

Positively charged ions (cations) negatively charged ions

(anions) are exchanged for hydrogen (H+) and hydroxyl
(OH-) ions, respectively, due to the resin’s greater
affinity for other ions.

The ion exchange process occurs on the binding sites of

the resin beads. 64
Q
 What is deionized water?
 What will be removed from the ion exchange
process?

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 What cannot be removed from ion exchange and
why?
 What are the application of deionized water?

65
 Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
TOPIC 2
Apparatus & Techniques
HEATING APPARATUS

Heating
apparatus

Electric Lab Bunsen Electric Microwave

Hotplate
Oven burner furnace Oven

Memmert
Lab Oven
drying oven

71
TYPES OF HEATING APPARATUS

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72
DESICCATORS OR DESICCANT DRY CABINET
 Vacuum dessicators Desiccant dry cabinet

73
 Desiccators or desiccant dry cabinet is an
enclosure with a supply of desiccant which
maintains an internal environment of 1-20% RH
(relative humidity)

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 Desiccant itself is defined as: A substance that
has a high affinity for water and is used as a
drying agent .
 Commercially, desiccant materials are supplied
as: Montmorillaonite clay, silica gel, molecular
sieve, calcium oxide, calcium sulfate and zeolite.

74
APPLICATIONS OF DESICCATORS

 Prevention and protection against all types of

oxidation (rust)
 The prevention of the growth of fungus on optics

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 The dry preservation of lab materials and
samples as well as the protection of MSDs
(moisture sensitive devices) in electronic
industry.

75
 Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
TOPIC 2
Apparatus & Techniques
FILTRATION APPARATUS AND TECHNIQUES

 Filtration is a technique used either to remove

impurities from a solution or to isolate any
solid.

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 The two type of filtration commonly used in
chemical labs are:
1. GRAVITY FILTRATION
2. VACUUM FILTRAION

77
GRAVITY FILTRATION
 FOLD THE PAPER INTO A CONE BY FIRST
FOLDING IT IN HALF, AND THEN IN HALF
AGAIN, AS SHOWN.

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78
FILTERING THE SOLUTION

 Support the glass funnel in a ring or place it in

the neck of an Erlenmeyer flask.

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79
 FLUTED FILTER PAPER

 Usually used to filter hot solution.

 Hot filtration helps to remove insoluble
impurities.

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80
 VACUUM FILTRATION
 Vacuum filtration is primarily used to collect a desired
solid, for instance, the collection of crystals in a
recrystallization procedure.

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 Vacuum filtration uses either a Buchner or a Hirsh
funnel.
 It is fater than gravity filtration, because the solvent or
solution and air is forced through the filter paper by the
application of reduced pressure.

81
VACUUM FILTRATION (FILTERING BY
SUCTION)

 Buchner funnel + filter papeer

 Other filtering devices: porcelain, glass
aluminium oxide

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82
VACUUM FILTRATION
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80
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82
 ZK_CHM421_2016
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83
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84
 ZK_CHM421_2016

85

[Link]
14
 Contents
1. Laboratory apparatus
2. Analytical balances
3. Weighing
4. Volumetric glassware
5. Distilled water & deionized
water
6. Heating apparatus
7. Filtration apparatus and
techniques
8. Titration apparatus and
techniques
TOPIC 2
Apparatus & Techniques
 TITRATION APPARATUS AND TECHNIQUES

 A titration is a method of analysis that will allow you

to determine the precise endpoint of reaction and
therefore the precise quantity of reaction in titration
flask.

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 Buret is used to deliver the second reactant to the
flask.
 Indicator is used to detect the endpoint of reaction.

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TITRATION APPARATUS AND TECHNIQUES

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92
 Titrant
 Analyte

 Titre

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94
CHEMICAL REAGENTS
 Purity of reagents has an important effect on the
accuracy of the chemical analysis

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Classifying
chemicals

Reagent grade (GR) Primary standard

grade (AnalaR)

95

Special-purpose
reagent chemicals
(Prepared for specific
application.E.g.
spectroscopic
solvents and HPLC
solvents)
CHEMICAL REAGENTS
1. Reagent grade
Reagent grade chemical conform to the minimum standards
set forth by the Reagent Chemical committee of the American
Chemical Society and are used wherever possible in analytical
work.

2. Primary Standard Grade:

Extraordinary purity is required for a primary standard.
Primary standard reagent is carefully analyzed and the assay
is printed on the container label. Generally equal to ACS
grade (≥95%) and is acceptable for food, drug, or medicinal
use and is suitable for use in many laboratory and
analytical applications.

3. Special-Purpose Reagent
Chemicals that have been prepared for a specific application.
Included among these are solvents for spectrophotometry and
high-performance liquid chromatography.
RULES FOR HANDLING REAGENTS AND
SOLUTIONS

 Select the best suitable grade of chemicals

available for analytical work. Pick the smallest
bottle to supply the desired quantity (prevent

ZK_CHM421_2016
wastage and overdue)
 Replace caps of the reagent bottle immediately
after use.
 Hold the stopper of the reagents bottles between
your fingers; never set a stopper on the table.
 NEVER RETURN ANY EXCESS REAGENTS
TO A BOTTLE.
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