The South African Breweries Section : 1.

6
Page : 1 of 8
BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

1. INTRODUCTION
a) Many analyses require that the sample's concentration is reduced (diluted) to a known
quantifiable level. Samples are furthermore treated and or reacted with chemical
preparation (reagents) of which the exact concentration must be known. In order to
achieve this with a high degree of precision/accuracy, volumetric equipment (flasks) are
used, as is discussed in this section.
b) In order to ensure an absolute sound volumetric preparation, it is equally important that
all the other "Techniques and Practices" in this manual (Vol. X - Section 1.0) are sound
and in place, for one technique is frequently used together with one or more of the others.
c) Temperature has a major impact on volume and therefore concentration of components in
a prepared solution.
Note: All preparations are made at 20 ± 0,2°C in our laboratories.
d) Volumetric flasks are used for:
i) Quantitative preparation of reagents, or
ii) Quantitative dilution of reagents and or samples.
e) These flasks are designed to either:
i) contain a specified volume, or
ii) deliver a specified volume.
Note: i) Delivery flasks (ID: ‘D’ or ‘TD’) are not used in our laboratories.
ii) Flasks intended to contain (ID: ‘C’, ‘TC’ or ‘IN’) are used for
preparations required in our laboratories.
f) Volumetric flasks are manufactured from high quality glass and graduated to contain a
specific volume under specified conditions.
Note: i) For all work in SAB laboratories, grade A glass volumetric flasks are
specified.
ii) DO NOT use grade B or plastic for quantitative preparations.
g) Polyethylene stoppers are used with these flasks.
h) References
i) SAB, Analytical MDT, 1995.
ii) Vogel’s, Textbook of Quantitative Inorganic Analysis, 4th Edition, 1978.
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BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

2. HEALTH AND SAFETY

2.1 HAZARDS
Broken glass can cause cuts, and when contaminated with chemicals a serious risk may
prevail.

2.2 SAFETY REQUIREMENTS

Do not dispose of broken glass in dust bins.

2.3 PRECAUTIONS
Wear protective gloves when clearing away broken glass.

3. APPARATUS
3.1 EQUIPMENT REQUIRED
a) Volumetric flask with stopper.
Flasks are available in the following general sizes 5, 10, 20, 25 50, 100, 250, 500, 1
000 and 2 000 ml. Odd sizes such as 1, 2, 3, 15, 30, 3 000 and 5 000 ml are
available.
Note: Only use grade A flasks graduated at 20°C (Temperature of graduation
is always shown on the flask).
b) Water bath set at 200,2°C.

3.2 EQUIPMENT PREPARATION

See Section 3.3.

3.3 EQUIPMENT MAINTENANCE

3.3.1 Volumetric Flask Cleaning
a) Flasks are washed in lukewarm water containing glassware detergent.
b) Rinse thoroughly with purified water, suspend upside down, allow to drain and
drip dry.
Note: Check for cleanliness. The purified water must drain evenly from
the inner wall without leaving behind droplets adhering to the
surface. Droplets are indicative of dirty spots.
3.2.2 General
a) Inspect the wall of the flask for cracks. If present, destroy the flask.
b) Should the inner wall become stained with chemicals or dye residues, they are
best removed as follows :
 Chemicals: soak in a mild acid i.e. 10% nitric or hydrochloric acid.
 Dyes: soak in ethanol.
Note: In both cases after the flask is washed, rinse and then soak in
purified water.
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BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

3.3 EQUIPMENT MAINTENANCE (Continued)

3.2.3 Golden Rules
Observation of these golden rules will ensure that the integrity of the flask’s
calibration remains sound and its accuracy and precision is maintained.
a) Wash in lukewarm solutions only.
b) Flasks (calibrated at 20°C) should not be subjected to temperatures < 15°C or
> 25°C and never to temperatures < 10°C or > 25 °C.
c) Volumetric flasks are washed immediately after use by the responsible
technician.
d) Flasks should not be washed in automatic glass washing machines unless the
operating temperature is set to below 25°C.
e) Flasks must not be used for storage of reagents.
Note: If required, they must be dedicated to this purpose and not used
elsewhere, likewise if the storage is in a refrigerator.
f) Do not dry volumetric flasks in an oven.
g) Preparations resulting in exothermic or endothermic reactions must not be made
in volumetric flasks.
- Exothermic reaction releases heat, the preparation warms up and can
become very hot.

e.g. H2SO4 + H2O  H3O+ + HSO4

- Endothermic reaction absorbs heat, the preparation cools down and can
become very cold.

e.g. NH4 NO2 + H2O  NH4OH + HNO2

h) Alkaline reagents (caustics) must be poured out of these flask immediately after
preparation. Caustic etches glass and adversely affects calibration status.

3.4 CALIBRATION

3.5 STORAGE
Store in a cupboard when not in use.

4. CHEMICALS
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BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

5. METHOD
5.1 PROCEDURE
a) Pre-attemperate sufficient purified water to 20  0,2°C.
b) Note specific requirements of the relevant method.
c) Quantitatively transfer the sample* to the flask.
*Can be :
- A fixed volume of sample (product being analysed).
- Fixed volume of a reagent or liquid chemical.
- Fixed mass of solid chemical or sample.
d) Fill the volumetric flask to about 85% of its capacity with pre-attemperated, purified
water and insert the stopper.
e) Mix to dissolve or to blend together.
f) Place in water bath and attemperate to 20 ± 0,2°C.
g) Remove the stopper and wash down into the flask.
Note: i) Avoid losing droplets.
ii) Place the stopper upside down on a clean surface.
h) Fill the flask to a level about 5-10 mm below the graduation mark with attemperated
purified water. Stopper, mix and stand in water-bath.
Note: i) Re-attemperate to 20 °± 0,2°C.
ii) Allow liquid to drain to below the graduation mark.
i) Using a pasteur-pipette add attemperated purified water and make-up to volume.
Note: Avoid parallax errors.
j) Re-stopper and mix well.

5.2 GOLDEN RULES - VOLUMETRIC PREPARATIONS

Adherence to these rules enhances accuracy and precision.
Liquid chemicals and/or solids may be transferred directly into the volumetric flask, and
about 85% of the required liquid (usually purified water), is added.
a) The ground glass stopper (or any other type) area must remain free from sample and
chemical.
b) When adding the purified water, the neck section above the graduation mark up to
just below the stopper section, must be thoroughly rinsed with the purified water.
c) It is normally better to pre-dissolve solids in a beaker, and then quantitatively
transfer the contents to the volumetric flask.
d) However, if diluting or dissolving takes place inside the flask in the “about 85%”
purified water, then mixing and shaking must be such that no liquid or solid is
shaken up to and into the neck area.
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BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

5.2 GOLDEN RULES - VOLUMETRIC PREPARATIONS (Continued)

e) When dissolved, fill to a level of about 5-10 mm below the graduation line
(depending on the flask size). Stopper and mix well.
f) Attemperate the flask and contents to 20°C. Partially loosen and lift (do not
remove) the stopper a few millimetres to allow any liquid to drain away from the
stopper down the neck of the flask.
g) Allow 15-20 seconds draining time, and carefully, with the aid of a dropper or
pasteur-pipette, correctly align the meniscus with the graduation mark. See next
step.
h) In order to make-up to the mark, it may be necessary to raise the flask to eye level.
To do this, the flask is held by the stopper area.
i) When working with a series of flasks containing different reagents or chemicals,
only one stopper at a time should be off, to avoid mixing them.
j) If it is absolutely necessary to simultaneously remove the stoppers from more than
one flask, they must be placed inverted on a clean piece of paper on the bench, in
such a way that they do not become mixed.
k) Following the preparation of a reagent it is immediately transferred to a reagent
bottle. The flask must be cleaned immediately. Likewise, on completion of the
tests in hand, the flask must be cleaned immediately, and packed away.

6. VERIFICATION
Fill a cleaned volumetric flask with purified water and drain. Check for absolute cleanliness,
that is, even drainage leaving no dry spots or water droplets on the inner wall of the flask, if
present, it is indicative of a dirty unclean flask.
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BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

7. COMPETENCY TEST

FORMATIVE ASSESSMENT CHECKLIST

Date : Candidate Name :

Position : Department Name :
Unit :
Element :
Assessor 1 : Assessor 2 :

Assessment 1 2 3

CHECKLIST COMPETENT NOT YET NOT

COMPETENT ASSESSED

1.0 PRODUCT
I’d know that the end product is right and as
manualised if:-
1. Dedicated flasks are clearly identified and
traceable.
2. Only grade ‘A’ volumetric glassware is used in
the laboratory.
3. A 'Change Management' record is in place and
current.
2.0 PROCESS
If the candidate did the job the correct way as
manualised he/she would:-
1. Adhere and comply to Health and Safety i.r.o.:
1.1 Cracked and chipped glassware are
hazardous.
1.2 Chemicals are hazardous.
3. Clean the volumetric flask:
3.1 With detergent.
3.2 With a 10% acid solution.
3.3 With a solvent.
3.4 Rinse with purified water (3x).
3.5 Inspect for damages.
4. Verify the cleanliness of the flask by observing
the drainage of purified water from the flask.
5. Attemperate purified water to 20 ± 0,2°C to use
in the preparation.
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BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

7. COMPETENCY TEST (Continued)

ASSESSMENT CHECKLIST (Continued)

CHECKLIST COMPETENT NOT YET NOT

COMPETENT ASSESSED

2.0 PROCESS (Continued)

6. Prepare a volumetric solution:
6.1 Quantitatively add the 'sample' to the flask.
6.2 Fill the flask to about 85% capacity with
attemperated purified water and stopper.
6.3 Mix to blend or totally dissolved.
6.4 Re-attemperate to 20 ± 0,2°C.
6.5 Fill the flask to 5-10 mm below the volume
mark with attemperated purified water and
mix.
6.6 Re-attemperate to 20± 0,2°C and verify
temperature.
6.7 Add attemperated purified water from a
dropper until the volume mark is matched.
6.8 Stopper the flask and mix thoroughly.
7. Adhere and comply to techniques and practices:
7.1 No sample or reagents on ground glass
stopper area.
7.2 Adding purified water in a manner to rinse
the neck section above the volume mark.
7.3 Only one flask and or reagent bottle with a
stopper removed.
7.4 Stopper or stoppers placed in a traceable
manner on clean paper.
7.5 Lift stopper slightly and allow liquid to drain
down and back into the flask before
removing it.
7.6 Verify that chemical salts are totally
dissolved prior to reaching the final volume.
7.7 Avoid parallax errors when making up to
volume.
7.8 Handle the volumetric flask only on the neck
area when making up to final volume.
8. Transfer (if a reagent) immediately to a reagent
bottle.
9. Clean volumetric flasks immediately after use
and return to storage.
 The South African Breweries Section : 1.6
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BREWING MANUAL 1st Issue : SEP 1996
Vol. X - Analytical Methods Rev. Date : OCT 1999

SECTION 1.6 : VOLUMETRIC PREPARATIONS

7. COMPETENCY TEST (Continued)

ASSESSMENT CHECKLIST (Continued)

CHECKLIST COMPETENT NOT YET NOT

COMPETENT ASSESSED

3.0 KNOWLEDGE
A candidate who does this job should be able to:
1. Describe and discuss the differences between
grade 'A and 'B' volumetric flasks.
2. Discuss the effect of temperature on volumetric
preparations.
3. Discuss the term 'Error of parallax'.
4. Discuss the term 'Quantitative'.
5. Explain the terms 'Exothermic' and 'Endothermic'.
6. Name five 'Golden Rules' you will observe in
order to protect and maintain the precision of a
volumetric flask.
7. Name two other volumetric apparatus used in a
laboratory

Competent : Not Yet Competent:

Comments :

Action Plan Follow up Dates

Assessor 1 Candidate
Sign. Sign.

Assessor 2
Sign.