( Reaffirmed 2004

)

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Indian Standard

METHODS OF CHEMICAL ANALYSIS OF STEELS
PART 12 DETERMINATION OF MANGANESE BY PERIODATE SPECTROPHOTOMETRIC METHOD IN PLAIN CARBON, LOW ALLOY AND HIGH ALLOY STEELS (FOR MANGANESE 0.01 TO 5.0 PERCENT)

( Fourth Revision)

ICS

77.080.20

0 BIS 2001

BUREAU
MANAK

OF

IN DIAN

STANDARDS

BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002
IMce Group 1

June 2001

low alloy and high alloy steels by periodate spectrometric method. observed or calculated. shall be rounded off in accordance with IS 2:1960 ‘Rules for rounding off numerical values (revised)’.01 to 1.01 to 0. expressing the result of a test or analysis.000 percent) Determination of copper by thiosulphate iodide method (for copper 0. MTD 2 FOREWORD This Indian Standard (Part 12) (Fourth Revision) was adopted by the Bureau of Indian Standards.05 to 2. IS 228. the final value. Determination of silicon by reduced molybdosilicate spectrophotometric in carbon steels and low alloy steels for silicon 0.25 percent) (third revision) Determination of molybdenum by thoicyanate (photometric) method in low and high alloy steels (for molybdenum 0.1 to 2 percent) Determination of oxygen by instrumental method Determination of nitrogen by steam distillation During this revision the method for determination of manganese in high alloy steels have been included and the periodate spectrometric method specified in the standard has been updated. The other parts of this series are: Part 1:1987 Part 2:1987 Part 3:1987 Part 4:1987 Part5 :1987 Part 6:1987 Part 7:1990 Part 8:1989 Part 9:1989 Part 10:1989 Part 11:1990 Part 13:1982 Part 14:1988 Part 15:1992 Part 16:1992 Part 18:1998 Part 19:1998 Methods for chemical analysis of steels — Determination of carbon by volumetric method (for carbon 0. For the purpose of deciding whether a particular requirement of this standard is complied with.50 percent) (third revision) Determination of manganese in plain carbon and low alloy steels by arsenite method (third revision) Determination of phosphorus by alkalimetric method (third revision) Determination of total carbon by gravimetric method (for carbon greater than or equal to 0. after the draft finalized by the Methods of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical Engineering Division Council.05 percent) (third revision) Determination of arsenic Determination of carbon by thermal conductivity method (for carbon 0. .05 to 5 percent) Determination of tungsten by spectrophotometric method (for tungsten 0. which was first published in 1952 and subsequently revised in 1959. covered the chemical analysis of plain carbon and low alloy steels along with pig iron and cast iron.05 to 0.1 percent) (third revision) Determination of nickel by dimethyl glyoxime (gravimetric) method (for nickel greater than or equal to 0. This part covers the method for determination of manganese in plain carbon. It was again revised to make it comprehensive in respect of steel analysis and to exclude pig iron and cast iron which were being covered in separate standards.1 percent) (third revision) Determination of molybdenum by alpha-benzoinoxime method (for molybdenum 1percent) (third revision) Determination of silicon by the gravimetic method (for silicon 0.50 percent) (third revision) Determination of sulphur in plain carbon steels by evolution method (for sulphur 0.005 to 2. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.5 percent) (third revision) .1 percent) (Wrd revision) Determination of chromium by persulphate oxidation method (for chromium greater than or equal to 0.Methods of Chemical Analysis of Ferrous Metals Sectional Committee.01 to 0. During its second revision the standard has been split up in several parts.

5 Potassium Periodate Solution Dissolve 7.1 Outline of the Method After dissolution of the sample in sulphuricphosphoric acid mixture and nitric acid. Store in a dark coloured glass stoppered bottle.1 mg Mn) Prepare as described in Method A or B.1 Method metal) A (Preparation from manganese IsNo. Heat to 55°C to 60°C and complete the titration by adding potassium permanganate solution until faint pink 1 5. constitute provision of this standard. 5.2. 264:1976 266:1993 1070:1992 3 SAMPLING Title Nitric acid (second revision) Sulphuric acid (third revision) Reagent grade water (third revision) The samples shall be drawn and prepared as described in the relevent Indian Standard specification.2.0 PERCENT) (Fourth Revision) 1 SCOPE This standard (Part 12) describes the method for the determination of manganese in plain carbon. phosphoric acid (rd=l . transfer to 1 litre volumetric flask. Add 400 ml of phosphoric acid. Let it stand in the dark for two weeks.2. 5. 70 percent.3 Perchloric Acid.8 percent) in a beaker and add 10 ml of dilute nitric acid (1 : 1).2. 4 QUALITY OF REAGENTS Unless specified otherwise. analytical grade reagents and reagent grade water (see IS 1070) shall be employed for the test.0 percent by periodate spectrophotometric method.4 Dilute Perchloric Acid. Manganese is oxidized to permanganic acid by potassium periodate. 2 REFERENCES The following Indian Standards contain provisions which through reference in this text.2. Add about 40 ml of potassium permanganate solution while stirring slowly.IS 228 (Part 12): 2001 Indian Standard METHODS FOR CHEMICAL ANALYSIS OF STEELS PART 12 DETERMINATION OF MANGANESE BY PERIODATE SPECTROPHOTOMETRIC METHOD IN PLAIN CARBON. LOW ALLOY AND HIGH ALLOY STEELS (FOR MANGANESE 0. At the time of publication.6. 5.84) (IS 266) and 150 ml of . 1:99 (v/v). Cool. 5 DETERMINATION OF MANGANESE Take 0. Avoid contact with rubber or other organic material. 5.2 g of potassium permanganate in 1 litre of water.2. 5. Transfer 0. 5.1 Sulplmric-Phosphoric Acid Mixture—Add 100 ml of sulphuric acid (rd=l . the solution is fumed with perchloric acid. Filter without washing through a Gooch crucible. Absorbance of the solution is measured at 545 nm. Add 250 ml of dilute sulphuric acid (1 : 19). Cool and dilute to 1 Iitre with water.01 to 5.01 TO 5. previously boiled for 10 to 15 min and then stir until the oxalate has dissolved.6.75) to 600 ml water.5 g of potassium periodate in 200 ml of dilute nitric acid (1 : 1) with warming. cool and dilute to 1 Iitre.6 Standard Manganese Solution (1 ml= 0.2 REAGENTS 5.6. 5.42) — Conforming to IS 264.2. Heat gently until dissolution is complete and brown fumes are expelled. and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below.1 g of manganese metal (purity 99.3 Standardization Dry a portion of sodium oxalate at 105° C.2. dilute to volume and mix.3000 g of sodium oxalate to 500 ml beaker. All standards are subject to revision .2.2 Nitric Acid (rd=l . 5. low alloy and high alloy steels in the range of 0. 5.2 Method B (Preparation from potassium permanganate) Dissolve 3. Let it stand until the pink colour disappears. the editions indicated were valid.

0. heat the solution at not less than 90”C for 20 to 30 min.2 Blank Carry out a blank by pipetting out another aliquot of the sample in a 250 ml conical flask. Cool and d~lute to volume. b) ~ 0. Dilute to volume and mix. mix.0. 4. where A B = = mass in mg. Add 10 ml HCI04.3.0 1. allow insoluble matter to settle and filter through a dry filter. Transfer 90 ml of 0.3. 1. add 50 ml water. evoporate to fumes to oxidize chromium and excess HC1.1 Select sample as per Table 1.3.20 percent. mass in g.2.5 1. Cool.4. Transfer 10 or 20 ml portions and specified in Table 1 to two 50 ml flasks.006 percent for manganese content below 0. To another add 10 ml nitric/phosphoric acid mixure. add 10 ml IU03 and heat to less than 90°C for 20 to 30 min.6) to seven 50 ml volumetric flasks and proceed according to 5.4 Calculation Manganese.02 to 0. Dilute to volume. Find out the normality of the solution and adjust to 0. 5.5 500 Add 8 to 10 ml HC1 (1 : 1).5. Add enough HN03 to hasten dissolution.5 Precision a) ~ 0.02 perc6nt. 2 .IS 228 (Part 12) :2001 colour persists for 30 s. percent by mass= $ x O. of the sample represented by aliquot of the solution taken.0 20 20 20 Transfer O. Add 5 ml of acid mixture (5. To one.05 to 0.5 >0. add 3 to 4 ml in excess. of manganese found aliquot of the solution. Table 1 Sample Selection Mn (%) (1) Weight (g) (2) Dilution (ml) (3) Aliquot (ml) (4) 0. Continue fuming till salts separate.1 N. Discard the first 15 to 20 ml filterate. 5. and in 10 10 0.100 or 500 ml flask.0 50 100 100 500 0. Reduce the potassium permanganate solution by sulphurous acid and boil the solution until free of sulphurdioxide.50 percent.5 to 5. Cool and proceed as in 5. digest transfer to a 50. Take the absorbance readings of first against second. Cool and transfer to 1 Iitre volumetric flask and make up. c) +0.1 to 0.0 1.3 Procedure 5.1 N potassium permanganate solution to 500 ml beaker and add 10 ml of dilute sulphuric acid (1 : 1). and d) *0. 5.0.1. Convert the spectrophotometeric readings of the sample to milligrams of manganese by means of calibration curve and calculate the percentage of manganese as given in 5.1) and boil for 10 min.00 percent.3. 2. 5.3. The dilutions and 2 The water used for dilution should be pretreated with potassium periodate.1.05 >0.50 to 2.0 ml of standard manganese solution (5.5 to 2. NOTES 1 A boiling water bath in which the flasks can be immerse~ may be used.20 to 0.01to 0.01 percent for manganese content between 0.5 >2. 5. 5.2.03 percent for manganese content between 0.02 percent for manganese content between 0.1 >0. 0. Draw a calibration curve of absorbance values against milligrams of manganese in the various aliquots.3 Calibration Curve alequots to be pipetted out are also given in Table 1.

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