Iso 3696 1987
Iso 3696 1987
Iso 3696 1987
Foreword
IS0 (the International Organization for Standardization) is a worldwide federation of
national standards bodies (IS0 member bodies). The work of preparing International
Standards is normally carried out through IS0 technical committees. Each member
body interested in a subject for which a technical committee has been established has
the right to be represented on that committee. International organizations, govern-
mental and non-governmental, in liaison with ISO, also take part in the work.
Printed in Switzerland
INTERNATIONAL STANDARD IS0 3696 : 1987 (E)
Grade 3
2 Description
Suitable for most laboratory wet chemistry work and prepara-
The material shall be a clear, colourless liquid as assessed by tion of reagents solutions; should be produced, for example, by
visual inspection. single distillation, by deionization, or by reverse osmosis.
Unless otherwise specified, it should be used for ordinary
analytical work.
3 Classification
NOTE - It is assumed that the initial feed stock water is potable and
This International Standard covers three grades of water as reasonably pure. If it is heavily contaminated in any respect, some
follows : pretreatment may be necessary.
Grade 1
1
IS0 3696 : 1987 (El
Table - Requirements
Grade 2 Test
Parameter Grade 1 Grade 3
method
pH value at 25 OC Not applicable Not applicable 5,0 to 7,5 Sub-clause 7.1
inclusive range (see note 1) (see note I)
Absorbance at 254 nm and 1 cm optical path length, 0,001 0,Ol Not specified Sub-clause 7.4
absorbance units, max.
NOTE - This sample is not used for measurements of conductivity on 7 Methods of test
grade 1 and grade 2 water (see 7.2.2.1).
It is essential that the determinations specified in this
The sample shall be placed in a suitable, clean, airtight con- clause are carried out in a dust-free, pure atmosphere and
tainer, reserved solely for water samples, which shall be of such that suitable precautions are taken to prevent any con-
a size that it is completely filled by the sample. Care shall be tamination of the sample and test portions.
taken to avoid the risk of contaminating the contents in any
way. 7.1 Measurement of pH
Aged containers (i.e. containers boiled for at least 2 h in a solu-
tion of hydrochloric acid, c(HCI) = 1 mol/l, then twice for 1 h 7.1.1 Apparatus
in distilled water) made of borosilicate glass can be used as well
as suitable inert plastics containers (for example polyethylene Ordinary laboratory apparatus and
or polypropylene), but it is essential to establish that the sample
is unaffected by storage therein, particularly in respect of pH-meter, fitted with a glass measuring electrode and an
oxidizable matter and absorbance. Ag/AgCI reference electrode.
7.1.2 Procedure
6 Storage
Calibrate the pH-meter (7.1.1) in accordance with the manufac-
Contamination of water during storage may arise principally turer’s instructions, using buffer solutions having pH values
from dissolution of soluble constituents from glass or plastics covering the range 4,0 to 8,0.
2
ISO3696:1987(E)
Transfer some of the laboratory sample to a suitable vessel and 7.3.2.2 Test
adjust the temperature of the water to 25 + 1 OC. Introduce
the electrodes and determine the pH. Add IO ml of the sulfuric acid solution (7.3.1 .l) and 1,O ml of
the standard volumetric potassium permanganate solution
(7.3.1.2) to the test portion (7.3.2.11, bring to the boil and boil
7.2 Measurement of conductivity for 5 min. Check that the colour of the test mixture is not com-
pletely discharged.
7.2.1 Apparatus
7.4 Measurement of absorbance
Ordinary laboratory apparatus and
7.2.1.1 Conical flask, fitted with a guard tube containing 7.4.1 Apparatus
self-indicating granular soda lime.
Ordinary laboratory apparatus and
NOTE - The limits are equivalent to oxidizable matter, expressed as Ordinary laboratory apparatus and
milligrams of oxygen (0) per litre, of 0,08 and 0,4 for grade 2 and grade
3 water respectively. 751.1 Rotary evaporator, with a flask of capacity about
250 ml.
7.3.1 Reagents
751.2 Steam bath.
Use grade 2 water to prepare the following reagent solutions.
7.5.1.3 Dish, of platinum, or borosilicate glass, of
7.3.1.1 Sulfuric acid, approximately 1 mol/l solution. capacity about 100 ml.
7.3.1.2 Potassium permanganate, standard volumetric 7.5.1.4 Oven, capable of being controlled at 110 + 2 OC.
solution, N/5 KMn04) = 0,Ol mol/l.
7.5.2 Procedure
7.3.2 Procedure
7.5.2.1 Test portion
7.3.2.1 Test portion
Transfer 1 000 ml of the laboratory sample into a stoppered
1 000 ml of grade 2 water or 200 ml of grade 3 water. measuring cylinder.
3
IS0 3696 : 1987 (El
Introduce 100 ml of the test portion into the clean and dry Transfer a 5,0 ml aliquot portion of the silica standard solution
rotary evaporator (7.5.1 .l) and distill on the steam bath (7.6.1 .l) to a 1 000 ml one-mark volumetric flask, dilute to the
(751.2) und er reduced pressure. As the water evaporates, add mark and mix.
successive quantities of the test portion until the entire test
portion has been evaporated to about 50 ml. 1 ml of this standard solution contains 0,005 mg of Si02.
Transfer the residue quantitatively to the dish (7.5.1.3), Prepare this solution at the time of use.
previously heated for 2 h in the oven (7.5.1.4) controlled at
110 + 2 OC, cooled in a desiccator and weighed to the nearest 7.6.1.3 Ammonium molybdate, 50 g/l solution.
0,000 1 g. Use two approximately 5 ml portions of the sample
to effect the transfer. Dissolve 5 g of powdered ammonium molybdate in a mixture of
80 ml of water and 20 ml of the sulfuric acid solution (7.6.1.5),
Using the steam bath, evaporate the residue to dryness. without heating. Store in a plastics bottle.
Transfer the dish and residue from the steam bath to the oven,
controlled at 110 I!I 2 OC, and leave for about 2 h. Remove the
dish from the oven, allow to cool to ambient temperature in a 7.6.1.4 IQ-Methyla ophenol sulfate (metal), indicator
desiccator and weigh to the nearest 0,000 1 g. Repeat the solution.
operation of heating, cooling and weighing until the difference
between two consecutive weighings does not exceed Dissolve 0,2 g of metol and 20 g of dipotassium disulfite
0,000 2 g. (potassium metabisulfite) in 100 ml of water, without heating.
Store in a plastics bottle.
75.3 Expression of results Discard the solution after 4 weeks, or if it shows prior signs of
decomposition.
The residue after evaporation and heating at 110 OC, expressed
7.6.1 .I Silica, standard solution I (concentrated). 7.6.2.1 Dish, of platinum, of capacity about 250 ml.
Weigh, to the nearest 0,000 1 g, 1 g of finely ground pure silica 7.6.2.2 Matched Nessler cylinders, of capacity 50 ml.
sand ( > 99,9 % of Si02), previously dried at 110 OC, into the
platinum dish (7.5.2.3). Add 4,5 g of sodium carbonate
7.6.2.3 Muffle furnace, capable of being controlled at 300 to
(anhydrous NazC03) and intimately mix the sample with a dry,
400 OC.
smooth-ended glass rod. Ease the mixture into the centre of the
dish and flatten it so that it covers an area about 30 mm in
diameter. Cover the mixture with a further 0,5 g of the sodium 7.6.2.4 Water-bath, capable of being controlled at approx-
carbonate, then gently brush any particles adhering to the glass imately 60 OC.
rod into the dish.
7.6.3 Procedure
Cover the dish with a platinum lid and place in the muffle fur-
nace (7.6.2.3), controlled at 300 to 400 OC. Heat the mixture,
7.6.3.1 Test portion
gradually raising the temperature for about 10 min or until
fusion is complete. Remove the dish from the furnace and
Take 520 ml of grade 1 water or 270 ml of grade 2 water.
gently swirl it to incorporate any particles. Allow to cool, wash
into the dish any particles adhering to the underside of the lid
with hot water, then dissolve the fused mass in hot water. 7.6.3.2 Test
Cool, transfer the solution quantitatively to a 1 000 ml one-
mark volumetric flask, dilute to the mark and mix. Evaporate the test portion (7.6.3.1) in the dish (7.6.2.1) in suc-
cessive portions, to produce a final volume of 20 ml. Add 1 ml
Transfer the solution to the plastics bottle for storage. of the ammonium molybdate solution (7.6.1.3). After exactly
5 min, add 1 ml of the oxalic acid solution (7.6.1.6) and mix
1 ml of this standard solution contains 1 mg of SiO,. well, After 1 min, add 1 ml of the metol solution (7.6.1.4), and
4
IS0 3696 : 1987 (E)
heat for 10 min in the water bath (7.6.2.41, maintained at ap- 8 Test reports
proximately 60 OC. Transfer the solution to one of the matched
Nessler cylinders (7.6.2.2). Each test report shall include the following particulars :
Prepare a standard colour solution following the same pro- a) an identification of the sample;
cedure, but using a mixture of 19,0 ml of the sample and 1,0 ml
of the standard silica solution (7.6.1.2) instead of the 20 ml b) the reference of the method used;
resulting from the evaporation of the test portion (7.6.3.1).
Transfer the solution to the other matched Nessler cylinder c) the results and the method of expression used;
(7.6.2.2).
d) any unusual features noted during the determination;
Viewing vertically downwards, check that the intensity of any
blue colour produced in the test solution does not exceed that e) any operation not included in this International Stan-
produced in the standard colour solution. dard, or regarded as optional.