GB/T 4701.5-1984 Chemical analysis methods for ferrotitanium - Periodate photometric method for determination of manganese content

GB/T 4701.5-1984 Chemical analysis method for ferrotitanium - Determination of manganese content by periodate photometry GB/T4701.5-1984 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of ferrotitaniumThe periodate photometric method for the determination of manganese content
Methods for chemical analysis of ferrotitaniumThe periodate photometric method for the determination of manganese contentThis standard is applicable to the determination of manganese content in ferrotitanium. Determination range: 0.10~1.50%. UDC 669.15' 295
-:543.4+546
CB 4701.5—84
This standard complies with GB1467-78 "General Principles and General Provisions of Standards for Chemical Analysis Methods of Metallurgical Products". 1 Summary of the method
The sample is dissolved in sulfuric acid and hydrochloric acid, titanium is oxidized with hydrogen peroxide, heated to emit sulfuric acid fumes, manganese is oxidized to permanganate with sodium periodaldehyde, and its absorbance is measured at a wavelength of 530nm on a spectrophotometer. 2 Reagents
2.1 Hydrogen peroxide (specific gravity 1.10).
2.2 Hydrochloric acid (1 - 1).
2.3 Sulfuric acid (1 + 1).
2.4 Sodium nitrate solution (10%). bzxz.net
2.5 Urea solution (10%).
2.6 Sodium periodate solution (5%).
2.7 Water without organic matter: Add 20ml of sulfuric acid (2.3) to 1000ml of water, heat to boiling, add a small amount of sodium periodate, continue to heat and boil for 10min, remove and cool to room temperature. 2.8 Manganese standard solution
2.8.1 Weigh 1.000g manganese metal (purity 99.9% 1), place in a 250ml beaker, add 20ml sulfuric acid (1+3), heat to dissolve, remove and cool to room temperature, transfer to a 1000ml volumetric flask, dilute to scale with water, and mix. This solution contains 1.0 g manganese per ml.
2.B.2 Transfer 10.00ml manganese standard solution (2.8.1), place in a 100ml volumetric flask, dilute to scale with water, and mix. This solution contains 0.1mg manganese per ml.
3 Instrument
Spectrophotometer.
The sample should pass through a 0.125mm sieve.
5 Analysis steps
5.1 Sample quantity
Weigh 0.5000g sample.
National Bureau of Standards 1984-10-04 Issued
1985-0901 Implementation
5.2 Blank test
Carry out a blank test with the sample.
GB 4701.5-84
5.3 Determination
5.3.1 Place the sample (5.1) in a 300ml beaker, add 20ml water, 20ml sulphuric acid (2.3), 10ml acid (2.2), blue Table III, heat until the sample is completely dissolved, remove the nitric acid and cool, add 5ml peroxide solution (2.1) in batches to oxidize titanium, etc. Then heat the sulfuric acid fume for 2-3min, remove and cool slightly, add 20ml hydrochloric acid (2.2), 50ml*, heat to dissolve the soluble salts, remove and cool to room temperature, transfer to a 100ml volumetric flask 1, dilute to the scale with water, and mix. 5.3.2 Filter the solution (5.3.1) through paper and discard the initial filtrate. Take 20.00ml of the filtrate and place it in a 200ml beaker. Add 10ml of sulfuric acid (2.3) and heat the sulfuric acid for 2-3min. Remove and cool slightly. Add 60ml of water and heat to dissolve the salts and boil for 2-3min. Add 10ml of sodium iodate solution (2.6) and continue to heat to boiling. When permanganate is generated, boil for another 5min to completely oxidize manganese to hydroxymanganic acid. Remove and cool to room temperature. Add 10ml of iodine solution (2.5) and transfer to a 100ml volumetric flask. Dilute to the mark with water (2.7) that does not contain organic matter and mix well. 6.3.3 Transfer part of the solution (5.3.2) to an appropriate colorimetric flask and measure its absorbance (A) at a distance of 530mm from the spectrophotometer using the sample as a reference. Take the remaining solution in the mouse bottle and add sodium nitrate solution (2.4) dropwise until the color of permanganate disappears completely. Shake for about 1 minute to make the bubbles disappear, transfer the solution into the appropriate colorimetric blood, and measure its absorbance (A2) under the same conditions as the previous one. The difference between the electrical absorbance A1 and A2 is used to calculate the true absorbance. Find the corresponding manganese content from the curve. 5.4 Drawing of the curve
Take 0, 1.00, 2.50, 5.00, 7.50, 10.00, 12.5%, and 15.00 ml of manganese standard solution (2.8.2) and place them in a group of 200 ml beakers. Add 15 ml of sulfuric acid (2.3) respectively, heat the sulfuric acid fume for 2 to 3 minutes, remove and cool slightly, add 60 ml of water, heat to dissolve the salt and boil for 2 to 3 minutes, add 10 ml of sodium periodate solution (2.6), continue to heat and boil, and when permanganate color is generated, boil for another 5 minutes to completely oxidize the manganese into manganic acid, remove and cool to room temperature, add 1 0ml of the bed element solution (2.5) is transferred into a 100ml volumetric flask, diluted to the mark with water (2.7) free of organic matter, and mixed. The following operations are carried out according to Section 5.3.3, and the absorbance is measured with the reagent blank as the reference, and the manganese content is used as the horizontal coordinate and the true absorbance as the vertical coordinate, and the curve is drawn as above. 6 Calculation of analysis results
Calculate the manganese content at each point according to the following formula:
The curve is drawn as above The manganese rats obtained above, g
sample, g:
test solution split ratio.
Analysis results are expressed to one decimal place. 7 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in the following table. Quantity
>0.50~1,00
>1.00-t,50
Additional explanation:
GB 4701.5a4
This standard is proposed by the Ministry of Metallurgical Industry of the People's Republic of China. This standard was drafted by Jinzhou Ferroalloys of the Ministry of Metallurgical Industry. From the date of implementation of this standard, the former Ministry of Metallurgical Industry Standard YB58165 "Chemical Analysis Method of Ferrotitanium" shall be used as the standard.
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