IS 228 Part 23
IS 228 Part 23
IS 228 Part 23
Indian Standard
METHODS OF CHEMICAL ANALYSIS OF STEELS
PART 23 DETERMINATION OF TOTAL NITROGEN IN STEEL BY OPTICAL
EMISSION SPECTROMETER ( NITROGEN 0.002 TO 1.0 PERC,ENT )
ICS 77.080.20
0 BIS 2003
FOREWORD
This Indian Standard ( Part 23 ) was adopted by the Bureau of Indian Standards, after the draft finalized by the
Methods of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical
Engineering Division Council.
1S 228, which was first published in 1952 and subsequently revised in 1959, covered the chemical analysis of plain
carbon and low alloy steels, alongwith pig iron and cast iron. It was revised again to make it comprehensive in
respect of steel analysis and to exclude pig iron and cast iron which were being covered in separate standards.
During its second revision the standard has been split up in several parts.
Determination of nitrogen in steel by steam distillation, has been covered in IS 228 ( Part 19) and Determination of
nitrogen in steel by inert gas fusion — Thermal conductivity method is under preparation and will be covered in
a separate standard which will form a part of the above series.
This part covers the method for determination of total nitrogen ( 0.002- 1.0 percent ) in steel by optical emission
spectrometer. The other parts of this series are:
(Part l): 1987 Determination of carbon by volumetric method ( for carbon 50 percent ) ( third
revision )
(Part 2): 1987 Determination of manganese in plain carbon and low alloy steels by arsenite method
( third revision)
(Part 4): 1987 Determination of total carbon by gravimetric method ( for carbon greater than or equal
to 0.1 percent ) ( third revision )
(Part 5): 1987 Determination of nickel by dimethyl glyoxime ( gravimetric ) method ( for nickel greater
than or equal to 0.1 percent ) ( third revision )
(Part 6):1987 Determination of chromium by persulphate oxidation method ( for chromium greater than
or equal to 0.1 percent ) ( third revision )
(Part 7): 1990 Determination of molybdenum by alphabenzoinoxime method ( for molybdenum greater
than 1 percent ) ( third revision )
(Part 8):1989 Determination of silicon by gravimetric method ( for silicon 0.05 to 0.50 percent ) ( third
revision )
(Part 9): 1989 Determination of sulphur in plain carbon steels by evolution method ( for sulphur 0.01
to 0.25 percent ) ( third revision )
(Part 10):1989 Determination of molybdenum by thiocyanate ( photometric ) method in low and high
alloy steels ( for molybdenum 0.01 to 1.5 percent ) ( third revision )
(Part n): 1990 Determination of total silicon by reduced molybdosilicate spectrophotometric method
in carbon steels and low alloy steels ( for silicon 0.01 to 0.05 percent) ( third revision )
(Part 12):1988 Determination of manganese by periodate spectrophotometric method in low and high
alloy steels ( for manganese 0.01 to 2.0 percent ) ( third revision )
(Part 14):1988 Determination of carbon by thermal conductivity method ( for carbon 0.005
to 2.000 percent)
(Part 15):1992 Determination of copper by thiosulphate iodide method ( for copper 0.05 to 5 percent )
Indian Standard
METHODS OF CHEMICAL ANALYSIS OF STEELS
PART 23 DETERMINATION OF TOTAL NITROGEN IN STEEL BY OPTICAL
EMISSION SPECTROMETER ( NITROGEN 0.002 TO 1.0 PERCENT )
3 PRINCIPLE OF THE TEST METHOD The optical emission spectrometer should be housed
in an air conditioned room maintained at a temperature
A capacitor discharge is produced between polished
specified by the manufacturer with a relative humidity
surface of the sample and a conical shaped electrode.
of 50 + 5 percent. The temperature should be kept
The discharge is terminated at a predetermined time.
within + 2°C of the nominal, to reduce the drift in spectral
The radiant energy of the nitrogen line and an internal
lines due to temperature variation. The room should
standard line are converted into electrical energy by
be free from vibrations, dust and oil vapours.
means of photomultiplier tubes. The concentration
of nitrogen in steel is obtained by reference to standard. 4.6 Counter Electrode
NOTE — The argon gas purifier system uses heated 5.2 Select 5 to 10 reference steel standards that cover
titanium, copper oxide and molecular sieves to absorb the required concentration range of nitrogen. Spark
1
1S 228( Part 23 ) :2003
these samples and construct the analytical curve as 7 ANALYSIS OF THE SAMPLE
per instructions in the operation manual of the
7.1 Place the prepared sample on the spark stand.
manufacturer of the instrument.
Spark the sample at two different spots. If the two
6 STANDARDIZATION values differ more than 3 standard deviations
established for procedure, then give a third spark.
6.1 Standardize the instrument as per the operation
Repolish and repeat the sparking at 2 or 3 spots. Take
manual of the manufacturer of the instrument. The
average of nearly matching values.
frequency of standardization will depend on the long
term stability of the instrument. 7.2 Spark a standard sample of known concentration
and make correction in the unknown sample result, if
6.2 Confirm that the standardization is correct by
necessary.
analyzing a standard sample. The value should be
within the allowable limits of the certified value of the NOTE — It is suggested that the standard sample used
standards. If not, repeat the standardization. for verification should have similar matrix and nearly
the same nitrogen content as the sample to be analyzed.
NOTE — The standardization should be repeated if the
argon cylinder has been changed, the spectrometer is 8 PRECISION
not in use for very long time or when an unusual drift
is noticed when a standard has been sparked for checking. The precision of analysis should be within *10 percent.
( (’ontinuedfrorn second cover)
(Part 21):1987 Determination of copper by spectrometric method ( for copper 0.02 to 0.5 percent )
( third revision)
( Part 24 ): 2003 Determination of nitrogen in steel by inert gas fusion — Thermal conductivity method
( nitrogen 0.001 to 0.2 percent)
In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or
calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off numerical
values ( revised )’.
Bureau oflndian Standards
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harmonious development of the activities of standardization, marking and quality certification of goods and
attending to connected matters in the country,
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copyright be addressed to the Director (Publications). BIS.
Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed
periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are
needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards
should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue
of’ ‘BIS Catalogue’ and ‘Standards : Monthly Additions’.
This Indian Standard has been developed from Doc : No. MTD 2 ( 4271 )
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