Glass alkalinity

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 Lecture 3(29-09-16)
learning objectives
• Explain how alkalinity develops in the glass?
• Describe the factors affecting alkalinity.
• Determine the effects of alkalinity on
Pharmaceutical dosage forms.
• "The capacity of water for neutralizing an
acid solution." - U.S. Geological Survey,
2010

• Alkalinity is a measure of the ability of a

solution to neutralize acids to the equivalence
point of carbonate or bicarbonate.
• Units: mEq/L (milliequivalent per liter).
• Commercially, ppm or parts per million.
• In all glass, the sodium and potassium oxides
are hygroscopic; the surface of glass absorbs
moisture from the air.
• Moisture and carbon dioxide in air causes the
Na2O  or NaOH and K2O or KOH to convert to
sodium (Na2CO3) or potassium carbonate (K2CO3)
which are extremely hygroscopic.
• In salt water, the Na+ and K+ carbonates in
unstable glass may leach out, leaving only
fragile, porous hydrated silica (SiO2 ) network.
This causes the glass to fade, crack, pit and
gives surface of glass a frosty appear.
• Large surface areas
• Long contact times with the atmosphere
Effect of Glass Alkalinity on
Pharmaceutical Products
• Use of buffered solution (stability retained)
• Use of unbuffered solution (stability lost)
• Borosilicate glass (stability retained)
• Soda lime glass (stability lost)
• Alkalinity of a solution is the capacity of it
to react with a strong acid (usually H2SO4)
to a predetermined PH.
• The alkalinity of a solution is usually made
up of carbonate, bicarbonate, and
hydroxides.
• Similar to acidity, the higher the alkalinity
is, the more neutralizing agent is needed
to counteract it.
•The scanning electron micrographs showed
surprising differences in the appearance of the
surface region.

Sulfur treatment of ampoules was associated with

a pitting (abrasions) of the surface and the
presence of sodium sulfate crystals.
The sulfur treatment of vials altered the glass
surface in a characteristically different way
Test of alkalinity of glass
Alkalinity testing(chemical test)
 1.Alkalinity test for whole glass
• Apparatus used:
Autoclave
Equipped with a thermometer, a pressure
gauge, a vent and a rack.
• Hardened-steel mortar and pestle.
o 8 Inch-sieves No. 20, 40 and 50 along with
the pan and cover
o 250ml conical flask and volumetric flask
made of resistant glass
• Special distilled water:
having a specific conductivity of 0.5 to1 Siemens.
• Methyl red solution:
Dissolve 24 mg of methyl red sodium in sufficient
purified water to make 100ml. if necessary,
neutralize the solution with 0.02 N NaOH.
• Take not less than 3 from each batch.
• Rinse twice the containers thoroughly with
distilled water.
• Fill each container to 90% of its overflow capacity
with the redistilled water.
• Cover the unsealed containers with crimped
pieces of new tin foil wash thoroughly with
acetone.
• Place the containers on in autoclave, close the
door, leaving the vent open.
• Heat until steam release vigorously from the vent
and continue heating for 10 min.
• Close the vent adjust the heating so that the
temperature rises 1°C/min until it reaches 121°C,
for 20- 25 min.
• Keep the temperature 121°C ± 0.5 °C for 1 hour.
• At the end decrease the supply of heat and cool
at the rate of 0.5 °C/min, until the internal
pressure is equal to the atmospheric pressure.
• Open the autoclave and allow the containers to
cool at 25 °C.
 • Titration:

Transfer 100 ml of water from each container add 5

drops of methyl red solution, and titrate with 0.01 N
sulphuric acid.
• The time elapsing between opening the
autoclave and titrating should not exceed 60
minutes.
• Carry out Blank Test on 100 ml of water from the
same lot, and make the necessary correction.

• The quantity of 0.01N sulphuric acid used for

containers with a capacity of up to 100 ml should
be, not more than 0.5 ml and for containers of
capacity greater than 100ml, not more than 1.5
ml.
2.Powdered glass test
• Take a clean dry empty glass containers 6 or
more.
• crush it in mortar-pestle.
• Crushing and sieving.
• Excess of 10g, stored in closed container in
desiccator.
• Spread the sample on butter paper.
• Remove the iron particles from sample.
• Transfer sample in a 250ml conical flask
• wash it with 30 ml acetone,
• swirling 30sec,and decant the acetone.
• Dry the contents in flask in oven at 1400C for
20 minutes.
• Transfer this powder in another dried conical
flask and cool in desiccator.
• add 50ml of distilled water. (sample
preparation)
• In another conical flask (100ml) add 50ml of
distilled water. (for blank reading)
• Cover both flasks with paper and place in
oven at 1210C for 30minutes.
• Cool them in desiccators.
• Transfer distilled water from sample
containing flask in another flask.
• Wash glass powder residues with 15 ml
special distilled water 4times and
• transfer this water in a flask contain main
portion
• add 5 drops of methyl red.
• Titrate against 0.02N H2SO4 until color
changes to light pink.

• Titrate the distilled water for blank

determination in the same way.

• Note: Blank reading should be 0.1-0.2ml and

sample reading should be 0.7-0.8ml.
3.Water attack test
• Rinse thoroughly 3 or more containers, twice with
special distilled water.
• Fill each container 90% capacity with distilled water.
• Follow procedure of powered glass test except the time
of autoclaving =1hour
• In a 250ml conical flask, transfer 100ml water from
each container, small container combine contents will
be use.
• 5drops methyl red indicator will be used
• Titrate with 0.02N H2SO4.(0.2ml-0.7ml)
• Titrate 100ml of special dis. water for blank titration.
• Wash the glass thoroughly in running tap
water and then soak it in distilled water.
• Dry the glass in two baths of alcohol. This
treatment will retard the disintegration and
also improves the appearance of the glass.
• It does not however, always stop the
breakdown of the glass.
• If applicable, apply an organic lacquer (PVA
or Acryloid B-72) to impede disintegration.
• For assurance, store the glass in a dry
environment with the relative humidity not
higher than 40 %.
• Parentral glass container: Sulphur treatment