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Specification for |
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Sulfuric acid used in |
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lead-acid batteries |
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ICS 29.220 : 71.060.30 |
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NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW
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BS 3031 : 1996
BSI 1996
Amendments issued since publication
First published September 1958 Amd. No. Date Text affected
Second edition March 1972
Third edition September 1996
Contents
Page
Committees responsible Inside front cover
Foreword ii
Specification
1 Scope 1
2 References 1
3 Definition 1
4 Description 1
5 Sample 1
6 Residue on ignition 1
7 Chloride content 1
8 Sulfur dioxide content 1
9 Ammoniacal nitrogen content 1
10 Nitrogen oxides content 1
11 Iron 2
12 Arsenic content 2
13 Copper content 2
14 Manganese content 2
15 Nickel content 2
16 Chromium content 2
17 Cadmium content 2
18 Test report 2
Annexes
A (normative) Calculation of conversion factor for each method 3
B (normative) Method for the determination of residue on ignition 3
C (normative) Method for the determination of chloride content 3
D (normative) Method for the determination of sulfur dioxide content 4
E (normative) Method for the determination of ammoniacal nitrogen content 5
F (normative) Method for the determination of nitrogen oxides content 6
G (normative) Method for the determination of iron content 7
H (normative) Method for the determination of arsenic content 8
J (normative) Method for the determination of copper, manganese,
chromium, nickel and cadmium by flame atomic absorption spectrometry 8
K (informative) Summary of specification requirements and conversions to
other acid concentrations 11
List of references Inside back cover
BSI 1996 i
BS 3031 : 1996
Foreword
This British Standard has been prepared by Technical Committee CII/8. It supersedes
BS 3031 : 1972, which is withdrawn.
This edition of BS 3031 incorporates specifications for nickel, chromium and cadmium
and the specifications for manganese have been revised. A flame atomic absorption
spectrophotometric method has been added for the determination of copper,
manganese, nickel, chromium and cadmium. This edition also introduces up-to-date
terminology.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.
ii BSI 1996
BS 3031 : 1996
Specification
1 Scope 5 Sample
This British Standard specifies the limits for A representative sample of not less than 1 l of the
impurities in sulfuric acid suitable for use in material shall be taken from the bulk. The sample
lead-acid batteries and details procedures for the shall be placed in a clean, dry and airtight stoppered
determination of those impurities. glass bottle of such a size that it is nearly filled by
This edition covers sulfuric acid of any relative the sample. When it is necessary to seal the bottle,
density. care shall be taken to avoid contaminating the
NOTE. This is a matter for agreement between purchaser and
contents in any way.
supplier. Clauses and relevant appendices are worded accordingly. The mass of test portion required for each test is
All of the numerical limits refer to sulfuric acid of given in the appropriate annex.
relative density 1.215 at 20 ÊC. Conversions to 100 % Since all numerical limits refer to acid having a
and other commonly used acid bases are given in relative density of 1.215 at 20 ÊC, all results obtained
annex K. Useful tables relating density to percentage on the sample of acid as received to their
composition will be found in BS 753 . equivalents, based on an acid of that relative density,
shall be converted by use of a conversion factor, F.
The calculation of the conversion factor is given in
2 References annex A.
2.1 Normative references
This British Standard incorporates, by reference, 6 Residue on ignition
provisions from specific editions of other
publications. These normative references are cited at When determined and calculated by the method
the appropriate points in the text and the described in annex B, the residue, on ignition of the
publications are listed on the inside back cover. material, shall not exceed the equivalent
Subsequent amendments to, or revisions of, any of of 150 mg´kg21 of the reference acid.
these publications apply to this British Standard only
when incorporated in it by updating or revision. 7 Chloride content
2.2 Informative references When determined and calculated by the method
This British Standard refers to other publications described in annex C, the chloride content of the
that provide information or guidance. Editions of material, expressed as CCl, shall not exceed the
these publications current at the time of issue of this equivalent of 7 mg´kg21 of the reference acid.
standard are listed on the inside back cover, but
reference should be made to the latest editions. 8 Sulfur dioxide content
When determined and calculated by the method
3 Definition described in annex D, the sulfur dioxide content of
For the purposes of this British Standard the the material, expressed as CSO2, shall not exceed the
following definition applies. equivalent of 5 mg´kg21 of the reference acid .
reference acid
Sulfuric acid of relative density 1.215 at 20 ÊC. 9 Ammoniacal nitrogen content
When determined and calculated by the method
described in annex E, the ammoniacal nitrogen
4 Description content of the material, expressed as CNH3, shall not
The material shall consist essentially of an aqueous exceed the equivalent of 50 mg´kg2 1 of the reference
solution of sulfuric acid, H2SO4, having a relative acid.
density not less than 1.215 at 20 ÊC. When diluted to
a relative density of 1.215 at 20 ÊC with water
conforming to Grade 3 of BS EN ISO 3696 : 1995, it 10 Nitrogen oxides content
shall be clear and colourless when viewed through a When determined and calculated by the method
depth of 300 mm. described in annex F, the nitrogen oxides content of
the material, expressed as CN, shall not exceed the
equivalent of 5 mg´kg21 of the reference acid.
BSI 1996 1
BS 3031 : 1996
15 Nickel content
When determined and calculated by the method
described in annex J, the nickel content of the
material, expressed as CNi, shall not exceed the
equivalent of 0.6 mg´kg21 of the reference acid.
2 BSI 1996
BS 3031 : 1996
Annexes
NOTE. 29.6 is the percentage by mass of H2SO4 in reference acid. C.2.3 Thirteen one-mark volumetric flasks,
conforming to BS 1792, 100 ml capacity.
Method for the determination of residue C.3.1 General. All reagents shall be of analytical
quality and water shall conform to Grade 3 of
on ignition BS EN ISO 3696 : 1995.
B.1 Apparatus C.3.2 Sulfuric acid, relative density 1.215 at 20 ÊC.
B.1.1 Platinum dish, approximately 50 mm in Add slowly, with constant stirring, 200 ml of sulfuric
diameter. acid, concentrated, 98 % (m/m), to 750 ml of water.
Cool to room temperature, then dilute to 1000 ml.
B.2 Procedure
Weigh to the nearest 0.01 g a test portion of C.3.3 Nitric acid, concentrated, approximately 70 %
approximately 50 g into the tared dish and evaporate to (m/m).
dryness on a sand bath in a fume cupboard until no C.3.4 Silver nitrate solution, approximately 17 g
further fumes are evolved. Finally ignite to constant AgN03 per litre.
mass at (850 ± 50) ÊC.
C.3.5 Standard chloride solution. Dissolve 1.648 g of
B.3 Calculation previously dried sodium chloride in water and dilute to
Calculate the residue on ignition, R, in percentage by 1000 ml. Mix well. Further dilute 10 ml of this solution
mass, using the equation: to 1000 ml with water. Mix well. 1 ml of this diluted
solution corresponds to 10 mg of Cl.
M2 3 100 3 F C.4 Procedure
R=
m C.4.1 Preparation of standard solutions
where Into 11 of the 100 ml one-mark volumetric flasks, each
containing 10 g (8.2 ml) of the sulfuric acid (C.3.2),
M2 is mass of residue found, in grams; transfer known amounts of the standard chloride
m is the mass of the test portion, in grams; solution (C.3.5), containing from 0 to 100 mg of
chloride increasing by stages of 10 mg and treat each
F is the conversion factor (see annex A). solution as follows.
Dilute to about 95 ml, add 1 ml of the nitric acid
Report the result as the mean of duplicate (C.3.3) and 2 ml of the silver nitrate solution (C.3.4),
determinations, to two significant figures. dilute to the mark with water, mix well and allow to
stand in the dark at room temperature, for not less
than 5 min and not more than 15 min.
These solutions are used directly for visual
comparison.
BSI 1996 3
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4 BSI 1996
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BSI 1996 5
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6 BSI 1996
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Add 1 ml of the 2,4-xylenol solution (F.3.5), mix well, G.2.2 Spectrophotometer, with 4 cm cells, or matched
insert the stopper and immerse the tube in the water Nessler cylinders conforming to BS 612.
bath (F.2.3) maintained at (35 ± 1) ÊC for 30 min. At
the end of this period, remove from the bath, transfer G.2.3 Fifteen one-mark volumetric flasks, conforming
the contents of the tube completely to the distillation to BS 1792, 100 ml capacity.
flask and dilute to 100 ml with water. G.3 Reagents
Connect the flask to the distillation assembly, heat to G.3.1 General. All reagents shall be of analytical
boiling and collect 60 ml of the distillate in a 100 ml quality and water shall conform to Grade 3 of
one-mark volumetric flask containing 10 ml of the BS EN ISO 3696 : 1995.
sodium hydroxide solution (F.3.6). Turn off the water
supply to the condenser towards the end of the G.3.2 Hydrochloric acid solution, approximately
distillation to ensure that no nitrated 2,4-xylenol 36.5 g HCl per litre.
remains in the condenser. Dilute to the mark with G.3.3 Hydroxylammonium chloride, 50 g/l solution.
water and mix thoroughly.
Carry out a blank test on 6.0 ml of the reagent sulfuric G.3.4 Ammonium acetate, 400 g/l solution.
acid (F.3.3), carefully adding it to 4.0 ml of water, G.3.5 2,2'-Bipyridyl, 1 g/l solution. Dissolve 0.1 g of
ensuring that the temperature does not rise the reagent in 50 ml of water containing 2 ml of the
above 40 ÊC. hydrochloric acid solution (G.3.2) and dilute to 100 ml.
Measure the absorbance of the test solution and that of
G.3.6 Standard iron solution. Dissolve 7.022 g of
the blank test solution at a wavelength of 445 nm using
diammonium iron(II) sulfate 6-hydrate in a mixture of
the dilute sodium hydroxide solution (F.3.6) as
600 ml of water and 350 ml of concentrated sulfuric
reference solution. Correct the absorbance of the test
acid solution, 98 % (m/m), and dilute to 1000 ml with
solution for that of the blank test solution and read the
water. Mix well. Further dilute 10 ml of the solution so
amount of nitrogen present from the calibration graph
obtained to 1000 ml with water. Mix well. 1 ml of the
(see F.4.2).
diluted solution corresponds to 10 mg of iron.
Alternatively, compare the colour of the two solutions
with the series of prepared colour standards in G.4 Procedure
matched Nessler cylinders, noting the nitrogen content G.4.1 Preparation of colour standards
of the standard that most nearly matches each
solution. Correct for the blank. Into 13 of the 100 ml one-mark volumetric flasks, each
containing 50 ml of water and 2 ml of the hydrochloric
F.5 Calculation acid solution (G.3.2), transfer known amounts of the
Calculate the nitrogen oxides content, CN, in standard iron solution (G.3.6), containing from 0 to
micrograms per kilogram, using the equation: 120 mg of iron, increasing by stages of 10 mg, and treat
M 3F each solution as follows.
CN = 5 Add 4 ml of the hydroxylammonium chloride solution
m
(G.3.3) and allow to stand for 1 min. Add 5 ml of the
where ammonium acetate solution (G.3.4) and 3 ml of the
2,2'-bipyridyl solution (G.3.5). Dilute the contents of
M5 is the mass of nitrogen found, in micrograms; each flask to 100 ml and mix thoroughly.
F is the conversion factor (see annex A); These standards are used directly for visual
m is the mass of the test portion, in grams. comparison. If an instrument is to be used, measure
the absorbance of each solution at a wavelength of
515 nm using the zero standard solution as reference
Report the result as the mean of duplicate standard, and prepare a calibration graph having, for
determinations to two significant figures. example, micrograms of iron as abscissa and
absorbance as ordinate.
Annex G (normative) G.4.2 Determination
Method for the determination of iron Weigh, to the nearest 0.01 g, a test portion of
content approximately 8 g containing not more than 120 mg Fe,
transfer it to a silica basin and evaporate just to
G.1 Principle dryness on a sand bath in a fume cupboard. Cool,
The iron present is reduced to the ferrous state and dissolve the residue in 2 ml of the hydrochloric acid
determined photometrically using 2,2'-bipyridyl. solution (G.3.2) and transfer to a 100 ml one-mark
volumetric flask.
G.2 Apparatus
G.2.1 Ordinary laboratory apparatus.
BSI 1996 7
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8 BSI 1996
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10 BSI 1996
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Annex K (normative)
Summary of specification requirements
and conversions to other acid
concentrations
Table K.1 gives a list of the limits specified on
reference acid (acid of relative density 1.215 at 20 ÊC)
and their conversion to an equivalent limit for
commonly used 100 %, 77 % and 50 % sulfuric acid.
Table K.1 Limits specified on reference acid (acid of relative density 1.215 at 20 ÊC ) and their
conversion to an equivalent limit for 100 %, 77 % and 50 % sulfuric acid
Impurity Limit specified on acid Equivalent limit for Equivalent limit for Equivalent limit for
of relative density 50 % H2SO4 relative 77 % H2SO4 relative 100 % H2SO4 relative
1.215 at 20 ÊC density 1.400 at 20 ÊC density 1.700 at 20 ÊC density 1.840 at 20 ÊC
mg´kg21 mg´kg21 mg´kg21 mg´kg21
Residue on ignition 150 275 424 550
Chloride 7.0 12 18 24
Sulfur dioxide 5.0 9 13 17
Ammoniacal nitrogen 50 85 131 170
Nitrogen oxides 5.0 9 13 17
Iron 12 21 32 41
Copper 7.0 12 18 24
Manganese 0.1 0.2 0.2 0.3
Arsenic 2.0 3.4 5.2 6.8
Nickel 0.6 1.0 2.0 2.0
Chromium 0.2 0.5 0.8 1.0
Cadmium 0.2 0.4 0.5 0.7
BSI 1996 11
12 blank
BS 3031 : 1996
List of references
Normative references
BSI publications
BRITISH STANDARDS INSTITUTION, London
Informative references
BSI publications
BRITISH STANDARDS INSTITUTION, London