INTERNATIONAL ISO

STANDARD 9280
First edition
1990-11-01

Water quality - Determination of sulfate -

Gravimetric method using barium chloride

iTeh STANDARD PREVIEW-

Qual&! de I eau - Uosage des sulfafes AMhode gravimktrique au
(standards.iteh.ai)
chlorure de baryum

ISO 9280:1990
https://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e-
a1e19ec86a89/iso-9280-1990

Reference number
ISO 9280: 199O(E)
ISO 9280:1990(E)

Foreword

ISO (the International Organization for Standardization) is a worldwide

federation of national Standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Esch 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. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an Interna-
tional Standard requires approval by at least 75 % of the member bodies
casting a vote. iTeh STANDARD PREVIEW
ISO/TC 147, Water quality.
(standards.iteh.ai)
International Standard ISO 9280 was prepared by Technical Committee

ISO 9280:1990
https://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e-
a1e19ec86a89/iso-9280-1990

0 ISO 1990
All rights reserved. No part of this publication may be reproduced or utilized in any form
or by any means, electronie or mechanical, including photocopying and microfilm, without
Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-1211 Geneve 20 l Switzerland
Printed in Switzerland

ii
INTERNATIONAL STANDARD ISO 9280:1990(E)

Water quality - Determination of sulfate - Gravimetric

method using barium chloride

iTeh STANDARD PREVIEW

(standards.iteh.ai)
1 Scope 3 Reagents
ISO 9280:1990
This Internationa! Standard specifies a gravimetric Use only reagents of recognized analytical
https://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e- grade
method for the determination of sulfate ina1e19ec86a89/iso-9280-1990
water. The and only distilled water or water of equivalent purity.
method is applicable to the analysis of all types of
water, including sea water and most industrial
3.1 Hydrochlorit acid, c(HCl)) = 6 mol/l.
effluents. For information on potentially interfering
substances, see clause 8. With care, mix 500 ml + 10 ml of concentrated
hydrochloric acid Cp(HCI)= IJ8 g/ml] with wate1
A sulfate concentration (expressed as SO:-) in the
and dilute to 1 litre in a measuring cylinder.
range of IO mg/l to 5000 mg/l tan be determined
using the specified test Portion (6.1). lt is possible to Store in a glass or polyethylene bottle. The Solution
determine higher concentrations after dilution of the is stable indefinitely.
Iaboratory Sample.
The lower limit of detection (with nine degrees of 3.2 Barium chloride, dihydrate solution, 100 g/l.
freedom) is
WARNING - Barium chloride is poisonous and
SO:- = 10 mg/l harmful if swallowed.

Dissolve 100 g + 1 g of barium chloride dihydrate

(BaCl,.2H,O) in about 800 ml of water, warming the
mixture to aid dissolution. Cool the solution and di-
2 Principle
lute to 1 litre with water in a measuring cylinder.
Acidification of the Sample with hydrochloric acid Store in a glass or polyethylene bottle. The Solution
followed by boiling with barium chloride solution for is stable indefinitely.
at least 20 min to promote coagulation of the pre-
cipitate of barium sulfate. Filtration through a tared
sintered-glass crucible, washing the precipitate free 3.3 Sodium hydroxide Solution,
from chloride, drying at 105 “C and reweighing when c(NaOH) = 5 mol/l.
cool. The increase in mass of the crucible is due to
the barium sulfate precipitate formed by reaction of WARNING - Sodium hydroxide solution is hazard,.
barium with sulfate ions in the Sample. ous on contact with skin and eyes.
ISO 9280:1990(E)

Dissolve 20,O g of sodium hydroxide in 100,O ml of NOTE 1 Samples low in organic matter may be kept for
water, whilst stirring. longer periods, but tests should be carried out to ensure
that samples are sufficiently stable.
Store in a polyethylene bottle.
5.2 Preparation of test Sample
3.4 Methyl orange, indicator Solution, about 1 g/l.
For the determination of sulfate in Solution allow any
Dissolve 100 mg of methyl orange in about 50 ml of suspended solids to settle Prior to withdrawing the
water, warming the mixture to aid dissolution. Cool test Portion (6.1). Alternatively, filter the laboratory
the Solution and dilute to 100 ml with water in a Sample through a fine porosity, ashless filter Paper
measuring cylinder. in Order to prepare a test Sample.
Store in a glass or polyethylene bottle. The Solution
is stable indefinitely. 6 Procedure

3.5 Silver nitrate Solution, about 0,l mol/l. 6.1 Test Portion
Dissolve 17 g +- 1 g of silver nitrate, AgNO,, in The test Portion volume shall be between IO ml and
about 800 ml of water and dilute to 1 litre in a 200 ml and shall contain not more than 50 mg of
measuring cylinder. sulfate ions. Using a pipette, withdraw the test por-
Store in an amber glass bottle. The Solution is stable tion from the settled test Sample (see 5.2).
indefinitely if protected from light.
NOTE 2 For shaken test samples containing large
amounts of suspended soiids it may be necessary to
3.6 Ethanol, CpH,OH, or rectified spirit (95 % measure the test Portion in a measuring cylinder, but with
ethanol, 5 % methanol). a likely consequent decrease in the accuracy and preci-
sion of the method.
3.7 Sodium chloride Solution,
iTeh STANDARD PREVIEW
100 g/l.

Dissolve IO,0 g + 0,l (standards.iteh.ai)

g of sodium chloride, NaCI,
6.2 Pretreatment

in about 100 ml ofwater. 6.2.1 Measure the test Portion (6.1) into a 500 ml
ISO 9280:1990
beaker and add 2 drops of methyl orange indicat.or
Store in a glass or polyethylenehttps://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e-
bottle.
(3.4). Neutralize the test Portion with hydrochloric
a1e19ec86a89/iso-9280-1990
acid (3.1) or sodium hydroxide Solution (3.3) de-
3.8 Sodium carbonate, Na,CO,, anhydrous. pending on the initial pH. Add 2 ml + 0,2 ml of
hydrochloric acid and then, if necessaryy add water
4 Apparatus to bring the total volume in the beaker to
200 ml + 20 ml. Boil the contents of the beaker for
at least 5 min.
4.1 Sintered-glass crucibles, of capacity about
30 ml, porosity value of 4. If the Solution is clear after boiling, proceed to 6.3.
If insoluble material is present, filter the hot mixture
4.2 Buchner flask, equipped with safety guard for through a fine porosity, ashless filter Paper and
vacuum filtration. wash the filter piper with a small amount of hot wa-
ter, combining the washing with the filtrate. Transfer
the Solution quantitatively to a 500 ml beaker and
4.3 Analytical balance, capable of weighing to at proceed to 6.3.
least 0,0002 g.
6.2.2 If it is suspected that the insoluble material
4.4 Platinum evaporating dish, of capacity 250 ml. retained by the filter Paper contains insoluble sulfate
and it is desired to include this in the final result,
5 Sampling and Sample preparation retain the filter Paper and carry out the’procedure
given in 9.2.
5.1 Sampling
6.2.3 If silica is present in the test Portion at con-
centrations likely to interfere (see clause 8), follow
Collect samples in glass or polyethylene bottles and
the pretreatment method given in 9.1.
analyze on the day of collection or store at 2 “C to
5 OC for not more than one week.
6.2.4 If organic substances are present in the test
Fill the Sample bottles completely to exclude air and Portion at concentrations likely to interfere (see
thus eliminate the risk of Oxidation of samples con- clause 8), follow the pretreatment method given
taining sulfide or sulfite. in 9.1.

2
 ISO 9280:199O(E)

ci.3 Precipitation 6.6 Blank test

Boil the Solution produced at the end of the pre- For a check of crucibles to be used in the test follow
treatment (6.2) and slowly add, using a pipette, a procedure identical to that given in 6.3 to 6.5, but
IO ml + 1 ml of hot (about 80 “C) barium chloride using 200 ml + 20 ml of water.
solutioc(3.2). Heat the Solution for at least 1 h, cover
and allow to cool and stand overnight at Subtract the crucible mass recorded before filtration
50 “C -+ IO “C. as in 6.4 from that recorded after filtration as in 6.5
to obtain the blank mass in grams.
NOTE 3 Slow addition of the hot barium chloride re-
duces the possibility of coprecipitation. Subsequent heat- NOTE 6 If filtration is necessary during Sample pre-
ing aids coagulation of the precipitate and renders it more treatment (6.2) the Portion of water used in the blank test
crystalline, reducing coprecipitation even further. shall fit-st be frltered as described in the second Paragraph
of 6.2.1, unless previous tests have demonstrated that no
contribution to the blank arises from filtration.

6.4 Filtration
7 Expression of results

6.4.1 Procedure
7.1 Calculation
Dry a sintered-glass crucible (4.1) by heating it to
105 “C for 1 h and let it cool in a desiccator. Calculate the mass of barium sulfate in the test
Sample, wt, in grams, from the following equation:
Accurately weigh the crucible (to the nearest
m = m2 - m, - q ...0
0,0002 g) and then fit it on a Buchner flask (4.2). Fil-
ter the precipitate using gentle suction. Use a
rubber-tipped iTeh STANDARDwhere
glass rod to dislodge any precipitate PREVIEW
remaining in the beaker and rinse with cold water
(standards.iteh.ai)
into the crucible. Wash the precipitate in the crucible
‘n, is the blank
in 6.6;
mass, in grams, calculated
with chloride-free cold water.
ISO 9280:1990 mf is the crucible mass, in grams, recorded
in 6.4;
https://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e-
6.4.2 Test for chloride in the washings a1e19ec86a89/iso-9280-1990
Hl2 is the crucible mass, in grams, recorded
in 6.5.
Collect about 5 mf of the filtrate from 6.4.1 in a stnall
beaker containing about 5 ml of silver nitrate sol- Calculate the sulfate concentration, in milligrams
ution (3.5). To ascertain whether the washings and per litre as SO:-- from the following equation:
hence the barium sulfate precipitate are free from
chloride, observe the mixture and check that no m x 1000 x 0,4116
. . . (2)
turbidity is formed. Otherwise continue washing. v

NOTE 4 lt is also important to check that no chloride where

remains on the rim of the underside of the crucible.
m is the mass of barium sulfate precipi-
tate, in grams;
V is the test Portion volume, in millili-
6.5 Drying and weighing tres (see 6.1);
Remove the crucible and dry it at 105 “C + 2 “C for 0,411 6 is the gravimetric factor.
about 1 h. Transfer the crucible to a desi&ator and
weigh it when it has cooled to room temperature so
that the mass is accurately known. Return the
crucible to the drying oven for a further IO min and Table 1 - Conversion factors for other units
repeat the cooling and weighing. Provided that the of concentration (c)
second mass differs by not more than 0,0002 g from
the first, record the second mass. Otherwise repeat
the drying, cooling and weighing until two succes-
sive masses do not differ by more than 0,0002 g.
SO:- = 1 mg/1 1 0,010 41 0,333 8
NOTE 5 Shorter drying periods may be obtained if the c(SO~-) = 1 mmol/l 96,06 1 32,06
precipitate is washed with three 5 ml portions of ethanol
(3.6).

3
ISO 9280:199O(E)

7.2 Precision 8 Interferences

Repeatability and reproducibility Standard devi- Sulfide and sulfite could interfere if samples arc lln-
ations have been determined as shown in table2. duly exposed to air causing Oxidation to sulfate to
occur before analysis. Othetwise, any sulfides and
sulfites present at the beginning of the analysis are
Table 2 - Repeatability and reproducibility removed as hydrogen sulfide and Sulfur dioxide
Standard deviations gases respectively, by boiling during pretreatment
(6.2).
Test Sulfate
Portion
volume
concen-
tration
cvr CVR Organic compounds present in substantial amounts
Sample (for example a Sample with a permanganate index
ml mg/1 mgll % mg/l % > 30 mg/l 0,) may interfere by absorption or co-
precipitation. Follow the procedure given in
1 200 50 313 clause 9 to overcome this difficulty.
2 20 210 313 1,6 69 3,3
3 20 583 814 L4 12,9 Zl Amounts in the test Portion (6.1) of other inorganic
4 20 1 160 93 W3 11,6 1,o ions, below which no interference is likely, are given
5 20 1 500 21,3 in table 3.
6 20 5 000 28,4

where
9 Special cases
Or is the repeatability Standard deviation;

cvr is the repeatability Variation coefficient; 9.1 Removal of organic compounds

% is the reproducibility
iTeh STANDARD
Standard deviation;
PREVIEW
Measure the test Portion (6.1) into a platinum evap-

CVR is the reproducibility (standards.iteh.ai)

Variation coefficient.
orating dish (4.4) and add two drops of methyl or-
ange indicator (3.4).
1,5,6: Standard solutions, data from United Kingdom, one ISO 9280:1990 Neutralize the test Portion with hydrochloric acid
(3.1) or sodium hydroxide (3.3) according to the ini-
laboratory, nine degrees ofhttps://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e-
freedom.
tial pH and then add 2,0 ml of hydrochloric
a1e19ec86a89/iso-9280-1990 acid.
2: Data from Germany, F.R., IO laboratories, 37 degrees Evaporate almost to dryness on a water bath and
of freedom. then add five drops of sodium chloride solution (3.7)
to the remaining liquid. Evaporate to complete
3: Data from Germany, F.R., IO laboratories, 35 degrees dryness and then heat the dish to a dull red heat
of freedom.
(about 700 “C) over a bunsen flame or in a muffle
furnace to form an ash.
4: Data from Germany, F.R., 9 laboratories, 32 degrees
of freedom. Allow to cool and then moisten the ash with about
IO ml of water. Add five drops of hydrochloric acid
(3.1) and evaporate to dryness on a water bath. Then
allow to cool slightly, add 3 ml rt: 1 ml of water and
warm the mixture in the basin to near boiling Point.
Then proceed as described in 6.2, beginning with
Y.. filter the hot mixture...” in the second Paragraph
Table 3 - Tolerante to other ions
of 6.2.1.
Maximum mass
in the test
Ions Expressed Portion 9.2 Determination of suifate in insoluble
material

Chromate CrOg- IO
9.2.1 Place the filier Paper from 6.2.2 in a platinum
Phosphate po;- IO dish (4.4) covered with a lid and either heat over a
low bunsen flame or place it in a muffle furnace at
Nitrate NO;- 100
room temperature and bring the muffle furnace up
Silicate SiOz- 2,5 to a temperature of 500 “C to burn off the Paper. Mix
the ignited residue with 4 g + 0,l g of anhydrous
Calcium Ca*+ 100
sodium carbonate (3.8) and he<t strongly to fuse the
Iron( Ill) Fe3+ 50 mixture, maintaining it in a melted state for 15 min.
Allow to cool.

4
 ISO 9280:i 990(E)

Add 50 mf of water to the platinum dish, warm to by drawing water through under s uction before dry-
dissolve the fused mixture and then filter the sol- ing and re-use in subsequ ent anal yses.
ution through a coarse filter Paper. Wash the filter
Paper with 20 ml of water. With the combined filtrate 11 Test report
and washings, proceed as described in 6.2 to 6.6,
beginning with “... add 2 drops of methyl orange in- The test report shall include the following informa-
dicator ...” in the first sentence of 6.2.1. tion:
Note that there is a st rong evolution of carbon diox-
ide when the acid is a dded a) a reference to this International Standard;

b) complete identification of the Sample;

9.2.2 Calculate the additional sulfate concentration,
SO:--, in milligrams per litre, as described in
c) the results, rounded to ? mg/1 (values befow
clause 7 and add it to the soluble sulfate concen-
100 mg/l), but not more than three significant
tration determined on the filtrate produced during
figures (values above 100 mg/l rounded to
pretreatment (6.2) to arrive at the total sulfate con-
10 mg/l) or precision data;
centration.
d) a Statement of the repeatability achieved;
10 Notes an procedure
e) details of the preparation of the test Sample (see
Cleaning of used sintered glass crucibles clause 5);
Barium sulfate tan be removed from the crucibles
after the analysis by soaking them overnight in a
9 whet her any of the special case procedures were
used
Solution containing about 5 g of disodium
ethylenediamine tetraacetate (EDTA, disodium sait)
and about 25 ml of ethanolamine iTeh STANDARDg)PREVIEW
[CH,(OH)CH,NH,]
any operations not specified in the method, or
regarded as optional, which might have affected
per litre of water. After soaking, wash the crucibies
the results or any other information relevant to
(standards.iteh.ai)
the procedure followed.

ISO 9280:1990
https://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e-
a1e19ec86a89/iso-9280-1990
ISO 9280:1990(E)

iTeh STANDARD PREVIEW

(standards.iteh.ai)
ISO 9280:1990
https://standards.iteh.ai/catalog/standards/sist/3dcf2b8d-9783-4fbb-bb2e-
a1e19ec86a89/iso-9280-1990

UDC 556.114:543.35:543.21 1
Descriptors: water, quaiity, Chemical analysis, determination of content, sulphates, gravimetric analysis.

Price based on 5 pages