GB/T 223.58-1987 PDF English
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Methods for chemical analysis of iron, steel and alloy - The sodium arsenite-sodium nitrite titrimetric method for the determination of manganese content
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GB/T 223.58-1987: Methods for chemical analysis of iron, steel and alloy - The sodium arsenite-sodium nitrite titrimetric method for the determination of manganese content
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT223.58-1987
GB
NATIONAL STANDARD
UDC 669.14/.15.543.06
Replacing the Method I in GB 223.4-81
Methods for chemical analysis of iron, steel and alloy -
The sodium arsenite-sodium nitrite titrimetric method
for the determination of manganese content
APPROVED ON. APRIL 03, 1987
Implemented on: MARCH 01, 1988
Approved by. Ministry of Metallurgical Industry
Table of Contents
1 Method summary... 3
2 Reagent... 3
3 Analytical procedures... 5
4 Calculation of analysis results... 7
5 Precision... 8
Appendix A Precision test raw data (Supplement)... 9
Additional information... 10
Methods for chemical analysis of iron, steel and alloy -
The sodium arsenite-sodium nitrite titrimetric method
for the determination of manganese content
This standard applies to the determination of the amount of manganese in pig
iron, carbon steel, alloy steel, and iron powder. Measuring range is 0.10% ~ 2.
50%.
This standard follows the requirements GB 1467-78 “Method for chemical
analysis of metallurgy product - General rules and regulations”.
1 Method summary
The sample is dissolved in acid; in the sulfuric acid and phosphoric acid
medium, the silver nitrate is used as catalyst AND the ammonium persulfate is
used to oxidize the manganese to septivalence, AND the sodium
arsenite-sodium nitrite standard solution is used for titration. Test solution
containing cobalt more than 5 mg will affect the observation of end point, AND
it may add nickel to offset the effect of the color of the cobalt ion.
2 Reagent
2.1 Nitric acid (ρ1.42g/ml).
2.2 Nitric acid (2 + 98).
2.3 Hydrochloric acid (ρ1.19g/ml).
2.4 Perchloric acid (ρ1.67g/ml).
2.5 Sulfuric acid (ρ1.84g/ml).
2.6 Sulfuric acid (2 + 3).
2.7 Hydrofluoric acid (ρ1.15 g/ml).
2.8 Ammonium hydroxide (ρ0.90g/ml).
2.9 Sulfuric acid-phosphoric acid mixture. slowly ADD 150ml of sulfuric acid
(2.5) and 150ml of phosphoric acid (ρ1.70g/ml) into 700ml of water; STIR it
continuously and COOL it down.
2.10 Sulfuric acid-phosphoric acid mixture. MIX the sulfuric acid (2.5),
phosphoric acid (ρ1.70g/ml) and water by equal volume; COOL it down.
2.11 Aqua regia. MIX three parts of hydrochloric acid (2.3) and one part of nitric
acid (2.1).
2.12 Silver nitrate solution (0.5%). WEIGH 0.5g of silver nitrate; DISSOLVE it
into water; ADD a few drops of nitric acid (2.1); USE water to dilute it to 100ml;
STORE it into a brown bottle.
2.13 Zinc oxide suspension. WEIGH 50g of zinc oxide; ADD 200ml of water;
STIR it during use.
2.14 Ammonium persulfate solution (20%). PREPARE it before use.
2.15 Sodium chloride solution (0.4%). WEIGH 4g of sodium chloride; USE
sulfuric acid (2.6) to dissolve it; and DILUTE it to 1l.
2.16 Potassium permanganate solution (0.16%).
2.17 Manganese standard solution.
2.17.1 WEIGH 1.4383g of benchmark potassium permanganate; PLACE it into
a 600ml beaker; ADD 30ml of water to dissolve it; ADD 10ml of sulfuric acid (1
+1). ADD hydrogen peroxide (ρ1.10g/ml) to the point when the red is just
disappeared; HEAT to boil it for 5 ~ 10 min; COOL it down; TRANSFER it into a
1000ml volumetric flask; USE water to dilute it to the mark; MIX it uniformly.
AND 1ml of this solution contains 500µg of manganese.
2.17.2 WEIGH 0.5000g of electrolytic manganese [99.99%, electrolytic
manganese treatment method. electrolytic manganese is placed into sulfuric
acid (5 + 95) for cleaning; after the surface manganese oxide is washed clean,
it is taken out and repeated rinsed by distilled water, then placed in the
anhydrous ethanol for washing for 4 ~5 times, and taken out and placed in the
drier for drying, before use]; PLACE it into a 250ml beaker; ADD 20ml of nitric
acid (1 + 3); HEAT to dissolve it; BOIL it to remove all nitrogen oxides; TAKE it
off and COOL it to room temperature; TRANSFER it into a 1000ml volumetric
flask; USE water to dilute it to the mark; MIX it uniformly; AND 1ml of this
solution contains 500µg of manganese.
2.18 Sodium arsenite-sodium nitrite standard solution. WEIGH 1.63g of
sodium arsenite and 0.86g of sodium nitrite; PLACE it into a 1000ml beaker;
USE water to dissolve and dilute it to 1000ml; MIX it uniformly.
Or otherwise WEIGH 1.25 ~ 1.30g of arsenic trioxide; PLACE it into a 1000ml
beaker; ADD 25ml of 15% sodium hydroxide solution; HEAT to dissolve it at
low temperature; USE water to dilute it to 200ml; ADD sulfuric acid (2.6) to
make the solution acidic and in excess of 2 ~ 3ml; then USE 15% sodium
carbonate solution to naturalize it to make the pH reach 6 ~ 7; ADD 0.86g of
sodium nitrite; USE water to dilute it to 1000ml; MIX it uniformly.
Calibration of sodium arsenite-sodium nitrite solution. WEIGH three parts of
iron (manganese content of not more than 0.002%) similar with the sample;
respectively PLACE it into 300ml conical flasks; ADD 30ml of sulfuric
acid-phosphoric acid mixture (2.9); HEAT to dissolve it; ADD nitric acid (2.1) to
destroy carbides; BOIL it to remove the nitrogen oxides; TAKE it off and COOL
it; respectively ADD manganese standard solution (manganese content similar
to the amount of manganese in the sample); USE water to dilute it to make the
volume reach about 80ml; FOLLOW the requirements of 3.2.2.The range
value of the millimeters of sodium arsenite-sodium nitrite solution as consumed
by the three solutions shall not be more than 0.05ml, AND the average value is
taken.
The titer of sodium arsenite-sodium nitrite standard solution for manganese is
calculated in accordance with the formula (1).
Where.
T - Titer of sodium arsenite-sodium nitrite standard solution for manganese,
g/ml;
V1 - Volume of manganese standard solution pipetted, ml;
V2 - Average value of volume of sodium arsenite-sodium nitrite standard
solution consumed for titration, ml;
C - Concentration of manganese standard solution, g/ml.
3 Analytical procedures
3.1 Sample amount
WEIGH the sample in accordance with Table 1.
Table 1
Manganese content, % Sample amount, g
0.10 ~ 1.00 0.5000
> 1.00 ~ 2.50 0.2500
3.2 Determination
3.2.1 Sample dissolution
3.2.1.1 Samples containing less than 5 mg of chromium
PLACE the sample (3.1) into a 300ml conical flask; ADD 30ml of sulfuric
acid-phosphoric acid mixture (2.9); HEAT to dissolve it; ADD nitric acid (2.1) to
destroy the carbide; BOIL to remove the nitrogen oxides. If the solution is still
containing black insoluble, it shall evaporate the solution to the point when the
sulfuric acid smoke is produced; carefully ADD 2ml of nitric acid (2.1) to
destroy the carbides; CONTINUE heating to produce sulfuric acid smoke until
the solution becomes clear; TAKE it off and COOL it down. USE water to dilute
it to make its volume reach to about 80ml.
Note. When the solution containing cobalt greater than 5mg, ADD nickel
solution at the ratio of one part of cobalt and four parts of nickel [WEIGH
47.85g of nickel sulfate (NiSO4 • 7H2O); USE water to dissolve it; ADD several
drops of sulfuric acid (2.5); USE water to dilute it to 100ml; AND 1ml of this
solution contains 10mg of nickel]; then DILUTE it to make the volume reach to
about 80ml.
3.2.1.2 Samples containing more than 5 mg of chromium
PLACE the sample (3.1) into a 300ml conical flask; ADD 10 ~ 20ml of aqua
regia (2.11); HEAT to dissolve it [as for high silicon sample, it may add several
drops of hydrofluoric acid (2.7)]; ADD 10ml of perchloric acid (2.4); HEAT to
evaporate it to produce smoke, until the trivalent chromium is oxidized to
hexavalent chromium; ADD hydrochloric acid (2.3) for several times; HEAT it
until smoke is produced every time after adding hydrochloric acid.
EVAPORATE it to make it reach to syrup state; TAKE it off and COOL it slightly;
ADD 15ml of sulfuric acid-phosphoric acid mixture (2.10) along the bottle wall;
HEAT to evaporate it until sulfuric acid smoke is produced for 1 ~ 1.5 min;
TAKE it off and COOL it down; ADD water to make its volume reach to about
80ml (SEE 3.2.1.1 when the cobalt content is more than 5mg).
The above steps can also be carried out in accordance with the following
method. WEIGH 0.5000 ~ 1.0000 g of sample; PLACE it into a 300ml conical
flask; ADD 10 ~ 15ml of aqua regia (2.11); HEAT to dissolve it [as for high
silicon sample, it may add several drops of hydrofluoric acid (2.7)]; ADD 10ml
of sulfuric acid (2.5); HEAT to evaporate it until sulfuric acid smoke is produced;
COOL it down; carefully ADD 100ml of water; HEAT to dissolve the salts; ADD
ammonium hydroxide (2.8) until a small amount of hydroxide precipitate is
produced; then ADD sulfuric acid (2.6) until the precipitate is dissolved;
TRANSFER the solution into a 250ml volumetric flask; ADD zinc oxide
suspension (2.13) for several times until a large amount of precipitation of
hydroxide appears, with an excessive amount of 15ml; after cooling it down;
USE water to dilute it to the mark; MIX it uniformly; FILTER it at dry state.
PIPETTE 100ml of filtrate; PLACE it into a 300ml conical flask; ADD 15ml of
sulfuric acid-phosphoric acid mixture (2.10).
3.2.1.3 Pig iron sample
PLACE the sample (3.1) into a 300ml conical flask; ADD 30ml of sulfuric
acid-phosphoric acid mixture (2.9); HEAT to dis...
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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