GB/T 223.62-1988_English: PDF (GB/T223.62-1988)
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Methods for chemical analysis of iron, steel and alloy - The butyl acetate extraction photometric method for the determination of phosphorus content
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GB/T 223.62-1988
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| Standard ID | GB/T 223.62-1988 (GB/T223.62-1988) | | Description (Translated English) | Methods for chemical analysis of iron, steel and alloy - The butyl acetate extraction photometric method for the determination of phosphorus content | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.08 | | Word Count Estimation | 5,550 | | Date of Issue | 1988/2/5 | | Date of Implementation | 1989/2/1 | | Older Standard (superseded by this standard) | GB 223.3-1981 | | Drafting Organization | Ministry of Metallurgical Industry | | Administrative Organization | Ministry of Metallurgical Industry | | Issuing agency(ies) | National Bureau of Standards | | Summary | This standard applies to pig iron, iron, carbon steel, alloy steel, high temperature alloys, precision determination of phosphorus content of the alloy. Measurement range 0. 001% to 0. 05%. |
GB 223.62-1988
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
UDC 669.14/.15. 543.06
H 11
GB 223.62-88
Replacing GB 223.3-81 Method III
Methods for Chemical Analysis of Iron, Steel and Alloy
- The Butyl Acetate Extraction Photometric Method
for the Determination of Phosphorus Content
ISSUED ON. FEBRUARY 05, 1988
IMPLEMENTED ON. FEBRUARY 01, 1989
Issued by. National Bureau of Standards;
Approved by. Ministry of Metallurgical Industry of PRC, January 18, 1988.
Table of Contents
1 Method Summary ... 3
2 Reagents ... 3
3 Analysis Procedures ... 5
4 Calculation of Analysis Results ... 8
5 Precision ... 8
Appendix A Original Data on Precision Test (Supplement) ... 9
Additional information... 9
Methods for Chemical Analysis of Iron, Steel and Alloy
- The Butyl Acetate Extraction Photometric Method
for the Determination of Phosphorus Content
This Standard is applicable to the determination of phosphorus content in pig iron, iron
powder, carbon steel, alloy steel, high-temperature alloy, precision alloy. The
measuring range is 0.001% ~ 0.05%.
This Standard complies with GB 1467-78 Method for Chemical Analysis of Metallurgy
Product – General Rules and Regulations.
This Standard complies with GB 7729-87 Chemical Analysis of Metallurgical Products
– General Rule for Spectrophotometric Methods.
1 Method Summary
In 0.65~1.63mol/l nitric acid medium, phosphorus and ammonium molybdate generate
phosphorus-molybdenum heteropoly acid, which is extracted by butyl acetate; use
stannous chloride to reduce and back-tract the phosphorus-molybdenum heteropoly
acid into aqueous phase; then measure the absorbance at the wavelength of 680nm.
The extraction solution contains the following amounts of elements like 2.5µg of
zirconium, 20µg of arsenic, 25µg of niobium, tantalum, 50µg of titanium, 500µg of
cerium, 1.5mg of tungsten, 2mg of steel, 3mg of cobalt, 5mg of chromium, aluminum,
and 50mg of nickel; which shall not interfere with the determination.
When the above limits are exceeded, the arsenic shall be removed by hydrochloric
acid, and hydrobromic acid; vanadium shall be reduced by ferrous; zirconium shall be
covered by hydrofluoric acid; after oxidizing into high price, the chromium shall be
removed by hydrochloric acid; in the EDTA ammoniacal solution, the tungsten shall
take beryllium as carrier, and precipitate the phosphorus; niobium, titanium, zirconium,
tantalum shall use copper and iron reagents, and chloroform to extract and remove.
2 Reagents
2.1 Oxalic acid. solid.
2.2 Copper and iron reagents. solid.
2.3 Boric acid. solid.
2.4 Butyl acetate.
2.5 Chloroform.
2.6 Hydrobromic acid (ρ 1.49g/ml).
2.7 Perchloric acid (ρ 1.67g/ml)
2.8 Hydrochloric acid (ρ 1.19g/ml)
2.9 Hydrochloric acid (1+5).
2.10 Nitric acid (1+2).
2.11 Nitric acid (1+2), it is prepared by boiling nitric acid (ρ 1.42g/ml), then remove
the nitrogen dioxide, and cooling off.
2.12 Sulfuric acid (1+2).
2.13 Hydrofluoric acid (1+10).
2.14 Ammonium hydroxide (ρ 0.90g/ml).
2.15 Ammonium hydroxide (1+50).
2.16 Ferrous sulfate solution (5%). every 100ml of solution contains 1ml of sulfuric
acid (1+1).
2.17 Sodium nitrite solution (10%).
2.18 Boric acid solution (2%).
2.19 Ammonium molybdate solution (10%).
2.20 Stannous chloride solution (1%). take 1g of stannous chloride (SnCl2•2H2O);
dissolve into 8ml of hydrochloric acid (2.8); dilute by water to 100ml; it shall be
prepared for current use.
2.21 Beryllium sulfate solution (2%). prepare with sulfuric acid (1+100).
2.22 Disodium ethylenediaminetetraacetic acid (EDTA for short) solution (10%).
2.23 Copper and iron reagent solution (6%).
2.24 Standard phosphorus solution.
2.24.1 Take 0.4393g of reference potassium dihydrogen phosphate (KH2PO4) (pre-
dried at 105°C to constant weight); dissolve by appropriate amount of water; add 10ml
of nitric acid (ρ 1.42g/ml); transfer into 1000ml volumetric flask; use water to dilute to
the scale; shake evenly. 1ml of such solution contains 100µg of phosphorus.
2.24.2 Pipette 20.00ml of standard phosphorus solution (2.24.1); place into 1000ml
volumetric flask; add 5ml of nitric acid (ρ 1.42g/ml); add water to dilute to the scale,
shake evenly. 1ml of such solution contains 2µg of phosphorus.
3 Analysis Procedures
3.1 Specimen quantity
Weigh the specimens as per Table 1.
Table 1
3.2 Blank test
Do the blank test accompanied by the specimen.
3.3 Determination
3.3.1 Specimen solution
3.3.1.1 General specimen
Place the specimen (3.1) into the conical flask; add nitric acid as per Table 1; heat and
dissolve [the insoluble specimen can be added 10~15ml of hydrochloric acid (2.8) for
assisting dissolving]; add perchloric acid as per Table 1; heat, vaporize and smoke till
the internal conical flask is transparent and back-flows for 5~6min (if the specimen
contains more than 2% manganese; add another 7~8ml of perchloric acid; vaporize
and smoke till the internal conical flask is transparent and back-flows for 20~25min);
vaporize till nearly dry; cool off.
3.3.1.2 Specimen with more-than-50g chromium content
According to the solution specimen in 3.3.1.1, vaporize till smoke; after chromium is
Content Range, %
Specimen quantity, g
Add nitric acid (2.10), ml
Add perchloric acid (2.7), ml
oxidized into hexavalent; add 2~3ml of hydrochloric acid (2.8) to volatilize chromium;
repeat the operation for 2~3 times; continue to vaporize till the internal conical flask is
transparent and back-flows for 3~4min; vaporize again till nearly dry; cool off.
3.3.1.3 Specimen with excessive-content of arsenic
Vaporize the solution specimen till smoke according to 3.3.1.1; cool off slightly; add
10ml of hydrochloric acid (2.8), 5ml of hydrobromic acid (2.6) to expel the arsenic;
continue to heat till the internal conical flask is transparent and back-flows 3~4min;
vaporize again till nearly dry; cool off.
3.3.2 Salts dissolvement and interfering elements treatment
3.3.2.1 General specimen
Add 30ml of nitric acid (2.10); heat and dissolve salts; titrate sodium nitrite solution
(2.17) till chromium is reduced to low-valent and continue to titrate for several
excessive drops; boiling it to remove nitrogen oxide; cool off to the room temperature.
Transfer the solution into 100ml volumetric flask; dilute with water to the scale; mix
evenly.
3.3.2.2 Tungsten-containing specimen
Use 20ml of water to dissolve the salts obtained from 3.3.1; add 10ml beryllium sulfate
solution (2.21), 10ml of EDTA solution (2.22), 2g of oxalic acid (2.1); use ammonium
hydroxide (2.14) to neutralize till pH is 3~4; dilute with water to about 90ml; boiling for
2~3min; then add 10ml of ammonium hydroxide (2.14); boiling for 1min; cool off to the
room temperature; filter the solution; wash by ammonium hydroxide (2.15); use water
to wash the precipitation into the original conical flask; add 30ml of nitric acid (2.10) to
dissolve the precipitation remained on the filter paper; discard the filter paper after
cleaning; then follows the procedures from titrating sodium nitrite solution (2.17) in
3.3.2.1.
3.3.2.3 Zirconium-containing specimen
Perform as per 3.3.2.1 till after cooling off to the room temperature; add 5ml of
hydrofluoric acid (2.13), shake evenly; add 20ml of boric acid solution (2.18); then
transfer the solution into 100ml volumetric flask; dilute with water to the scale; mix
evenly.
3.3.2.4 Specimen containing titanium, niobium, zirconium, tantalum
Add 10ml of water and 15ml of sulfuric acid (2.12) to dissolve the salts obtained from
3.3.1; titrate sodium nitrite solution (2.17) to reduce to hexavalent chromium; then
boiling and remove the nitrogen oxide; take off; add 5ml of hydrofluoric acid (2.13)
when it is hot; shake evenly; cool off to the room temperature. Transfer the solution
into 100ml volumetric flask; dilute with water to the scale; mix evenly.
Transfer 10.00ml of specimen solution to place into 60ml separating funnel; add
0.4~0.8g of copper and iron reagents (2.2), 20ml of chloroform (2.5); vibrate for 1min;
after standing and layering, discharge the organic phase; add 1ml of copper and iron
reagent solution (2.23), 10ml of chloroform (2.5) into aqueous solution; vibrate for 40s;
after standing and layering, discharge organic phase; then add 10ml of chloroform
(2.5); vibrate for 30s; after standing and layering, discharge organic phase [if the
copper and iron reagent has not been cleaned completely yet, then use chloroform
(2.5) to clean again]; add 0.04~0.1g of boric acid (2.3), 1ml of nitric acid (2.11); vibrate
for 10~15s. Then follow the procedures from adding 15ml of butyl acetate (2.4) in
3.3.3.2.
NOTE. for the specimen containing tungsten, titanium, niobium, tantalum, zirconium, firstly,
treat the tungsten-containing specimen; then treat the specimen containing titanium, niobium,
tantalum, zirconium.
3.3.3 Coloration
3.3.3.1 Transfer 10.00ml of specimen solution from the solution obtained from 3.3.2.1
or 3.3.2.2 or 3.3.2.3 into 60ml separating funnel.
3.3.3.2 Add 2~3 drops of ferrous sulfate solution (2.16) (not adding into solution in
3.3.2.2), 15ml of butyl acetate (2.4), 5ml of ammonium molybdate solution (2.19) into
separating funnel; ...
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