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2:1994
STANDARDS AUSTRALIA
1 The Crescent,
Homebush NSW 2140 Australia
PREFACE
This Standard was prepared by the Joint Australia /New Zealand Standards Committee
CH/10 on Analysis of Metals, to supersede AS 1050.2—1984, Methods for the analysis of
iron and steel, Part 2: Determination of carbon content (gravimetric method).
It is issued as part of a Joint Standard under the terms of the Active Cooperation
Agreement between Standards Australia and Standards New Zealand.
CONTENTS
Page
1 SCOPE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
2 REFERENCED DOCUMENTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
3 PRINCIPLE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
4 REAGENTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
5 APPARATUS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
6 SAMPLING AND SAMPLES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
7 PROCEDURE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
8 CALCULATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
9 PRECISION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
10 ACCEPTANCE OF ANALYTICAL VALUES . . . . . . . . . . . . . . . . . . . . . . . . . 7
11 TEST REPORT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
APPENDIX
A SET UP OF APPARATUS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1 SCOPE This Standard sets out a gravimetric method for the determination of the
total carbon content of all types of iron and steel, after combustion in oxygen using a high
temperature resistance furnace or high frequency induction heating. The method is
applicable to all types of iron and steel with carbon contents in the range 0.05% to 4.5%.
4 REAGENTS
4.1 General requirements Only reagents of recognized analytical grade and only
distilled water or water of an equivalent purity shall be used.
4.2 Manganese dioxide, for combustion analysis Particle size range from 710 µm to
1.18 mm.
4.3 Magnesium perchlorate, anhydrous
4.4 Carbon dioxide absorbent Inert granular base impregnated with sodium
hydroxide.
4.5 Glass wool
4.6 Accelerator The accelerator shall be either lead, red lead, tin or tungsten
containing less than 0.001% carbon.
NOTES:
1 Red lead should be heated for several hours at 450°C to 480°C and transferred to a small
glass-stoppered bottle for storage. It should be reheated at 450°C to 480°C if it is stored for
several hours.
2 Metallic accelerators such as lead, tin or tungsten should be washed in a low boiling point
(<50°C) hydrocarbon and dried before use.
4.7 Oxygen Oxygen at least 99.5% pure with a minimum amount of carbonaceous
material.
4.8 Sulfuric acid (ρ20 1.84 g/mL).
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7 PROCEDURE
7.1 Number of determinations This method is written for a single determination only
and may be used in that form. Where replicate determinations are required, procedures for
the acceptance of results obtained are given in Clause 10.
7.2 Blank test A blank test shall be carried out in parallel with the analysis using the
same procedure as for the analysis and the same quantities of all reagents but omitting the
test sample.
7.3 Check test In each run one analysis of a certified reference material of the same
type of metal should be carried out in parallel with the analysis of the test sample and
under the same conditions. However, in cases of dispute, an analysis of a certified
reference material shall be carried out in parallel with the analysis of the test sample.
When the analysis is carried out on several samples of the same type of metal at the same
time, the analytical value of one certified reference material may be used.
NOTE: The certified reference material should be of the same type as the sample to be analysed
and the properties of the two materials should be sufficiently similar to ensure that in either
case no significant changes in the analytical procedure would become necessary.
7.4 Test portion Weigh to ±0.2 mg the test portion masses specified in Table 1.
TABLE 1
MASSES OF TEST PORTIONS
Carbon content Mass of test portion
% g
0.05 to 0.5 2.728
0.5 to 1.0 1.500
1.0 to 1.5 1.000
1.5 to 5.0 0.500
7.5 Determination
7.5.1 Combustion using a resistance furnace The procedure for combustion using a
resistance furnace shall be as follows:
(a) Set up the apparatus as shown in Figure A1.
(b) Adjust the furnace temperature to between 1050°C and 1100°C and regulate the
oxygen flow at between 300 mL/min and 325 mL/min.
(c) After 15 min detach the absorption bulb (5.4(d)) and weigh to the nearest 0.2 mg.
Replace the bulb and continue passage of oxygen for a further 15 min. Detach and
weigh the absorption bulb to the nearest 0.2 mg. Repeat the passage of oxygen and
weighing until the absorption tube reaches constant mass (difference between
successive weighings less than 0.5 mg). Record the mass (m1 ).
(d) Weigh a suitable test portion selected from Table 1 into a pre-ignited combustion
boat (5.6).
(e) Cover the test portion with approximately 1 g of accelerator (4.6).
NOTE: Some types of high chromium nickel steels require an additional aid to combustion,
e.g. the sample may be mixed with an equal mass of iron of known carbon content
(<0.005% carbon) in a similar state of dispersion to the test sample. When low carbon iron
is added as a combustion accelerator, a blank test should be carried out using the same
amount of iron and accelerator and the appropriate correction made.
(f) Bypass the oxygen stream through the mercury safety valve (5.1(d)).
(g) Attach the weighed absorption bulb (7.5.1(c)) and introduce the combustion boat
containing the test portion (7.5.1(d)) into the hot zone of the combustion tube (5.3).
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Allow the boat to preheat for 3 min in the hot zone of the combustion tube and then
readmit the oxygen (4.7).
(h) Rapid combustion begins approximately 1 min after introduction of the oxygen and
is indicated by a reduced oxygen flow. Continue the oxygen flow for 10 min after
combustion has been completed (i.e. after the oxygen flow rate returns to its
original value) and reweigh the absorption bulb to the nearest 0.2 mg after the bulb
has reached ambient temperature. Record the mass (m 2).
7.5.2 Combustion using an induction furnace The procedure for combustion using an
induction furnace shall be as follows:
(a) Set up the apparatus as shown in Figure A1.
(b) Adjust the oxygen flow to approximately 1 L/min.
(c) Weigh the absorption bulb to constant mass by the procedure specified in
Clause 7.5.1(c). Record the mass (m1 ).
(d) Weigh a suitable test portion, selected from Table 1, into a cupulet or crucible.
Cover the test portion with approximately 1 g of accelerator (4.6).
NOTE: Some types of high chromium nickel steels require an additional aid to combustion,
e.g. the sample may be mixed with an equal mass of iron of known carbon content
(<0.005% carbon) in a state of dispersion similar to the test sample. When low carbon iron
is added as a combustion accelerator, a blank test should be carried out using the same
amount of iron and accelerator and the appropriate correction made.
(e) Open the furnace and position the cupulet on the pedestal. Close the furnace
ensuring that the cupulet is in the correct position within the heating zone.
(f) Sweep the system with oxygen for approximately 30 s.
(g) Open the stopcock of the absorption bulb and connect it to the absorption train.
(h) Turn on the power switch of the furnace, record the time (if an automatic timer is
used, adjust it for a 5 min burning period) and burn the sample for 5 min.
(i) Continue the oxygen flow for 5 min after the furnace has been turned off and
reweigh the absorption bulb to the nearest 0.2 mg after the bulb has reached
ambient temperature. Record the mass (m 2).
8 CALCULATIONS
Calculate the carbon content of the sample from the following formula:
where
m2 = mass of absorption tube after combustion of test portion, in grams
m1 = mass of absorption tube prior to combustion of test portion, in grams
mb = mass of carbon dioxide in blank, in grams
m = mass of test portion, in grams
0.2729 = conversion factor converting carbon dioxide to carbon
9 PRECISION A planned trial of this method was carried out by five analysts, each
from a different laboratory, five tests being carried out by each analyst on each of six
samples. From the results obtained the 95% confidence limits (2s) have been calculated
in accordance with BS 4237 and the repeatability, r, and reproducibility, R, have been
calculated in accordance with AS 2850 . These data are presented as Table 2.
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TABLE 2
PRECISION DATA FOR CARBON DETERMINATIONS
Carbon Mean Components of
Reproducibility
certificate carbon standard Repeatability Reproducibility
Sample index
value content deviation
% % sb sw 2s r R
SRM 170 A 0.052 0.052 0.002 0.002 0.005 0.0056 0.0071
Basic open
hearth mild
steel
SAA 81/3 0.105 0.006 0.006 0.017 0.0168 0.0241
Carbon steel
SAA 81/5 0.513 0.007 0.015 0.033 0.0420 0.0467
Valve steel
(Cr 21, Mn 9,
Ni 4)
SAA 81/6 Tool 1.48 0.003 0.010 0.021 0.0280 0.0297
steel (Cr 12,
Mo 0.8, V 0.9)
SRM 6F 2.91 2.90 0.042 0.033 0.107 0.0924 0.1514
Cast iron
JSS 110/6 4.15 4.06 0.076 0.010 0.156 0.0280 0.2207
Pig iron
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(a) Where the difference between duplicate results is greater than r, a further
determination should be carried out. All three results may be accepted if the range
of results is less than 1.2r, otherwise a fourth determination should be carried out.
(b) Where the range of four results is less than 1.3r, all may be accepted. If the range is
greater than 1.3r, but three of the four results are within a range of 1.2r, these three
may be accepted and the fourth rejected. Should neither condition apply, a fifth
determination should be carried out.
(c) When the range of the five results is less than 1.4r, all may be accepted. Otherwise,
if four of the five results lie within the range of 1.3r, these may be accepted and the
fifth rejected.
(d) Where an outlier is obtained from four or five determinations, it may be rejected but
it is invalid to reject any result on the basis of only three determinations or to reject
two results from five determinations.
(e) Should five results fail to achieve acceptability according to the above scheme, a
detailed investigation should be made into all aspects of the analytical procedure,
including instrument performance, operator technique, sample homogeneity and
preparation.
The test result finally reported is usually the mean of all acceptable results. Acceptance of
this final result is, however, conditional upon the acceptability of the result obtained for
the reference material, where such a material has been carried through the method with
the test samples.
10.3 Acceptance of reference material values If the value obtained for the reference
material does not agree to within 0.7R of its recognized value, the procedure shall be
repeated with the original and a different reference material. Test sample results shall be
acceptable when the criteria of the above clause are met, and the value of the reference
material agrees to within 0.7R of its recognized value.
11 TEST REPORT
The test report shall contain the following information:
(a) Identification of the sample.
(b) Date on which the sample was taken.
(c) Date on which the analysis was carried out.
(d) Carbon concentration in the test sample, expressed as a percentage by mass of the
sample.
(e) Identification of the reference material, if used, to validate the result.
(f) Any alternative standardization procedure used to validate the test result.
(g) The number of acceptable results from which the mean result has been calculated.
(h) Reference to this Australian/New Zealand Standard, i.e. AS/NZS 1050.2.
(i) Any unusual observations made during the course of the analysis which may have
had an effect on the result.
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APPENDIX A
SET UP OF APPARATUS
(Normative)
LEGEND:
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