BRITISH STANDARD BS 3762-3.

13:
1983
ISO 6835:1981
CONFIRMED
JUNE 1993

Analysis of formulated
detergents —
Part 3: Quantitative test methods —

Section 3.13 Method for determination

of total boron content
[ISO title: Surface active agents — Washing powders —
Determination of total boron content — Titrimetric method]

NOTE It is recommended that this Section be read in conjunction with the information
in the “General introduction”, published separately as BS 3762-0.

UDC 661.185:543.24:546.27
BS 3762-3.13:1983

This British Standard, having

been prepared under the
direction of the Chemicals
Standards Committee, was
published under the
authority of the Board of BSI
and comes into effect on
30 December 1983
Amendments issued since publication
© BSI 12-1999

The committees responsible for Amd. No. Date of issue Comments

this British Standard are
shown in Part 0.
The following BSI references
relate to the work on this
standard:
Committee reference CIC/34
Draft for comment 80/51140 DC

ISBN 0 580 13558 6

 BS 3762-3.13:1983

Contents

Page
National foreword ii
1 Scope and field of application 1
2 References 1
3 Principle 1
4 Reagents 1
5 Apparatus 1
6 Sampling 2
7 Procedure 2
8 Expression of results 2
9 Test report 3
Table 3
Publications referred to Inside back cover

© BSI 12-1999 i
BS 3762-3.13:1983

National foreword

This Section of BS 3762 has been prepared under the direction of the Chemicals
Standards Committee. It is identical with ISO 6835:1981 “Surface active
agents — Washing powders — Determination of total boron content — Titrimetric
method”, published by the International Organization for Standardization (ISO).
This method supersedes method D2 of BS 3762:1964. The original method
involved isolation of the inorganic material in a test portion [by low temperature
ashing or by repeated extraction with 95 % (V/V) ethanol], dissolution in water,
treatment with anionic and cationic exchange resins to obtain the boric acid
present in the test portion and titrimetric determination with sodium hydroxide
solution in the presence of mannitol using phenolphthalein as indicator. The
revised method removes silicates by adjusting the original sample solution to
pH 3 and filtering, and then removes anionic-active matter and phosphates by
anion-exchange on a chloride form of resin. The boric acid is finally titrated
potentiometrically with sodium hydroxide solution in the presence of mannitol.
Terminology and conventions. The text of the International Standard has
been approved as suitable for publication as a British Standard without
deviation. Some terminology and certain conventions are not identical with those
used in British Standards; attention is drawn especially to the following.
The comma has been used as a decimal marker. In British Standards, it is current
practice to use a full point on the baseline as the decimal marker.
Wherever the words “International Standard” appear, referring to this standard,
they should be read as “Section of this British Standard”.
Cross-references
International Standard Corresponding British Standard
ISO 607:1980 BS 3762 Analysis of formulated detergents
Part 1:1983 Methods of sample division
(Identical)
ISO 1042:1981 BS 1792:1982 Specification for one-mark volumetric
flasks
(Identical)
The Technical Committee has reviewed the provisions of ISO/R 385 and ISO 648,
to which reference is made in clause 5, and has decided that they are suitable for
use in conjunction with this standard.
Related British Standards to ISO/R 385 and ISO 648 are, respectively, BS 846
“Specification for burettes” and BS 1583 “One-mark pipettes”.
Additional information
Reagents. With reference to clause 4, water complying with BS 3978 “Water for
laboratory use” is suitable.
With reference to 4.8 and its footnote, resins of this description from most
chemical suppliers have been found suitable. In 4.8 the term “rate of reticulation
of” may be ignored and it should be noted that the specified particle size
range 150 to 300 4m is approximately equivalent to the now superseded
designation “50–100 mesh” (see Appendix C of BS 410:1976 “Specification for test
sieves”).
Apparatus. With reference to the footnote to 5.9 and 5.10, many commercial types
have been found suitable and are readily available.
This standard describes a method of test only and should not be referred
to as a specification defining limits of purity. Reference to the standard
should indicate that the method of test used is in conformity with
BS 3762-3.13.

ii © BSI 12-1999
 BS 3762-3.13:1983

A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.

Compliance with a British Standard does not of itself confer immunity

from legal obligations.

Summary of pages
This document comprises a front cover, an inside front cover, pages i to iv,
pages 1 to 4, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on the
inside front cover.

© BSI 12-1999 iii

iv blank

1 Scope and field of application
This International Standard specifies a titrimetric
method for the rapid determination of the total
boron content of commercial washing powders,
without interference from other compounds usually
present.
The method may be used in the presence of
sequestering agents.
2 References
ISO/R 385, Burettes.
ISO 607, Surface active agents and detergents —
Methods of sample division.
ISO 648, Laboratory glassware — One-mark
pipettes.
ISO 1042, Laboratory glassware — One-mark
volumetric flasks.
3 Principle
Removal of phosphates from an aqueous solution of
a washing powder by passing over an ion-exchange
resin, followed by formation and titration of the
boric acid-mannitol complex.
4 Reagents
During the analysis, use only reagents of recognized
analytical grade, and only distilled water or water of
equivalent purity.
4.1 D-mannitol
4.2 Hydrochloric acid, 100 g/l solution.
Place 25 ml of hydrochloric acid
(Õ20 approximately 1,18 g/ml) in a 100 ml volumetric
flask, dilute to volume and mix.
4.3 Hydrochloric acid, 10 g/l solution.
Place 10 ml of the hydrochloric acid solution (4.2) in
a 100 ml volumetric flask, dilute to volume and mix.
4.4 Sodium hydroxide, 100 g/l solution.
Dissolve 10 g of sodium hydroxide in water in
a 100 ml volumetric flask, dilute to volume and mix.
4.5 Sodium hydroxide, 10 g/l solution.
Place 10 ml of the sodium hydroxide solution (4.4)
in a 100 ml volumetric flask, dilute to volume and
mix.
4.6 Boric acid, solution containing 0,5 g of boron
oxide (B2O3) per litre.
1)
A suitable resin is available commercially. Details may be obtained from the Secretariat of ISO/TC 91 (AFNOR) or ISO Central
Secretariat.
2)
Suitable apparatus is available commercially. Details may be obtained from the Secretariat of ISO/TC 91 (AFNOR) or ISO
Central Secretariat.
© BSI 12-1999
BS 3762-3.13:1983
Weigh, to the nearest 0,1 mg, 0,888 g of boric
acid (H3BO3), dissolve it in water in a 1 000 ml
volumetric flask and dilute to volume.
1 ml of this solution corresponds to 0,5 mg of boron
oxide.
4.7 Sodium hydroxide, standard volumetric
solution, c(NaOH) . 0,05 mol/l.
4.7.1 Standardization
By means of a pipette (5.3), place 25,0 ml of the
boric acid solution (4.6) in a 150 ml beaker,
add 75 ml of water, and proceed as specified
in 7.2.3.
4.7.2 Calculation of concentration
The concentration, c, expressed in moles of NaOH
per litre, is given by the formula
0,012 5
c = --------------------------------
V 0 ´ 0,034 8
where V0 is the volume, in millilitres, of sodium
hydroxide solution used for the titration of 0,012 5 g
of boron oxide.
4.8 Anion-exchange resin, strongly basic,
(quaternary ammonium group), (Cl–) form, with a
rate of reticulation of 4 % of divinylbenzene, and of
particle size range 150 to 300 4m.1)
5 Apparatus
Ordinary laboratory apparatus, and in particular:
5.1 Beaker, made of polyethylene, of
capacity 2 000 ml.
5.2 Volumetric flasks, of capacity 250 and 1 000 ml,
complying with the requirements of ISO 1042.
5.3 Pipettes, of capacity 25 and 200 ml, complying
with the requirements of ISO 648.
5.4 Burette, of capacity 10 ml, complying with the
requirements of ISO/R 385.
5.5 pH-meter, provided with an extended scale,
accurate to 0,05 pH unit.
5.6 Glass electrode
5.7 Calomel electrode
5.8 Ion-exchange column, of length 30 cm, internal
diameter 1,5 cm, with a reservoir of capacity 75 ml.
The column shall be filled with the resin (4.8) to a
length of 22 cm.
5.9 Vacuum filter, of capacity 250 ml.2)
5.10 Filter medium, high retention filter paper or
equivalent.2)
1
BS 3762-3.13:1983
5.11 Mechanical stirrer
5.12 Magnetic stirrer
6 Sampling
The washing powder laboratory sample shall be
prepared and stored in accordance with ISO 607.
7 Procedure
7.1 Test portion
Weigh, to the nearest 0,01 g, about 10 g of the
laboratory sample.
7.2 Determination
7.2.1 Preparation of the test solution
Transfer the test portion (7.1) to the beaker (5.1).
Fill the 1 000 ml volumetric flask (5.2) to volume
with water at 35 to 40 °C, and pour the water on to
the test portion, allowing a few seconds for drainage.
Stir vigorously, by means of the stirrer (5.11), for
about 3 min in order to dissolve the test portion.
Small quantities of insoluble silicates (and other
salts) may remain undissolved.
7.2.2 Separation by anionic exchange resin
By means of a pipette (5.3), transfer 200 ml of the
test solution (7.2.1) to a 250 ml beaker and, using
the hydrochloric acid solutions (4.2 and 4.3), adjust
the pH to 3 ± 0,1, checking by means of the
pH-meter (5.5) fitted with the glass electrode (5.6)
and the calomel electrode (5.7). Transfer this
solution quantitatively to the 250 ml volumetric
flask (5.2) and dilute to volume.
Transfer 50 ml of this solution to the vacuum
filter (5.9) and filter through the filter
medium (5.10); the filtrate shall be as clear as
possible to avoid any subsequent blocking.
Wash the filled ion-exchange column (5.8) with
water until the washings are neutral. By means of a
pipette (5.3), transfer 25 ml of the filtrate to the
reservoir of the column and allow it to flow through
the column at a rate of 1 to 1,5 ml/min, collecting
the eluate in a 150 ml tail-form beaker. Wash the
column three times with 25 ml portions of water,
allowing the water to flow at a rate
of 1 to 1,5 ml/min, and collect the washings in the
beaker.
Regenerate the resin after each passage of the test
solution by passing 100 ml of hydrochloric acid
solution diluted (1 + 4), [1 volume of hydrochloric
acid (Õ20 approximately 1,18 g/ml) + 4 volumes of
water], at a rate of 1 to 1,5 ml/min, and washing
with water, at the same rate, until the washings
have a pH equal to or greater than 5.
When not in use, the column should be filled with
hydrochloric acid solution diluted (1 + 4).
2 © BSI 12-1999
7.2.3 Titration
By means of the magnetic stirrer (5.10), stir the
eluate in the beaker and adjust the pH
to 5,80 ± 0,05, checking by means of the
pH-meter (5.5) fitted with the electrodes (5.6
and 5.7), using, as appropriate, the hydrochloric
acid solutions (4.2 and 4.3), or the sodium hydroxide
solutions (4.4 and 4.5). Add 12 g of the
D-mannitol (4.1).
After stirring for 1 min, titrate with the sodium
hydroxide solution (4.7), using the burette (5.4),
until a pH of 5,80 ± 0,05 is obtained, measured
using the normal scale, then the extended scale, of
the pH-meter.
The volume of the sodium hydroxide solution used to
return to the initial pH of 5,8 corresponds to the
quantity of boric acid present in the aliquot portion.
8 Expression of results
8.1 Method of calculation
The boron oxide content, expressed as a percentage
by mass, is given by the formula
V ´ c ´ 0,034 8 1 000 250 V ´ c ´ 174
--------------------------------------- ´ --------------- ´ ---------- ´ 100 = -----------------------------
m 200 25 m
where
V is the volume, in millilitres, of the sodium
hydroxide solution (4.7), used for the titration of
the 25 ml aliquot portion of the test
solution (7.2.1);
c is the exact concentration, in moles of NaOH
per litre, of the sodium hydroxide solution (4.7);
m is the mass, in grams, of the test
portion (7.1);
0,034 8 is the mass, in grams, of boron oxide
corresponding to 1 ml of exactly 1 mol/l sodium
hydroxide solution.
By replacing c in the above formula by the
expression given in 4.7.2, one obtains the formula
V ´ 62,5
----------------------
V0 ´ m
 BS 3762-3.13:1983

8.2 Precision
Comparative analyses, on samples of two washing
powders containing respectively 10 % (m/m) of
perborate [about 2 % (m/m) of B2O3] and 25 % (m/m)
of perborate [about 5,7 % (m/m) of B2O3] carried out
in eight laboratories, have given the statistical
results given in the following Table.
Table
Boron oxide content 2 % (m/m) 5,7 % (m/m)

Standard deviation of
0,05 0,08
repeatability, Ör
Standard deviation of
0,14 0,08
reproducibility, ÖR

9 Test report
The test report shall include the following
information:
a) all information necessary for the complete
identification of the sample;
b) the reference of the method used (reference to
this International Standard);
c) the results and the method of expression used;
d) the test conditions;
e) any details not specified in this International
Standard or in the International Standards to
which reference is made, or regarded as optional,
as well as any incidents likely to have affected the
results.

© BSI 12-1999 3
4 blank
 BS 3762-3.13:1983

Publications referred to

See national foreword.

© BSI 12-1999
BS 3762-3.13:
1983
ISO 6835:1981 BSI — British Standards Institution
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