Rapid analysis method for various elements in carbon steel
Determination of Mn, Si and P in Conventional Carbon Steel and Low-alloy Steel (Rapid Before Boiler): Determination of Manganese (Silver Salt - Ammonium Persulfate Oxidation Spectrophotometry):
First, the main reagent
1, nitric acid - silver nitrate (0.4%): In (1 + 4) diluted nitric acid 1000ml, add 4g of silver nitrate; 2, ammonium persulfate solution (15%);
Second, the analysis operation: Weigh 40mg in a 250ml high beaker, add 10ml of nitric acid - silver nitrate solution, heated to dissolve, add 5ml of ammonium persulfate solution, boil 10S, remove, add 40ml, shake, at a wavelength of 530nm Place, 2cm cuvette, water reference, measure the absorbance. Determination of silicon (ferrous reduction - silicon molybdenum blue photometric): First, the main reagent 1, nitric acid (1 +4); 2, potassium permanganate solution (5%); 3, alkaline ammonium molybdate solution: said Take 5g of ammonium molybdate, add 12.5g of potassium carbonate, dissolve, dilute to 100ml; 4, oxalic acid solution (2.5%) 5, ferrous ammonium sulfate solution (1%): Add 1ml of concentrated sulfuric acid per 100ml of solution.
Second, the analysis operation: Weigh the sample 30mg in a 250ml high beaker, add nitric acid (1 +4) 10ml, heated to the sample dissolved, shake the yellow gas away, add 3 drops of potassium permanganate solution, heated to Boiling, remove, immediately add 10ml alkaline ammonium molybdate solution, shake 10 seconds, add 40ml oxalic acid solution, 40ml ferrous ammonium sulfate solution, shake, at a wavelength of 660nm, 0.5cm cuvette, water reference, Measure absorbance. Determination of Phosphorus (sodium fluoride - stannous chloride - Phosphomolybdenum blue photometric method): 1. Main reagent 1, nitric acid (1+2.5); 2, potassium permanganate solution (5%); 3, ammonium molybdate (10%) - Potassium sodium tartrate (10%) (1+1 mixed on the same day); 4, sodium fluoride - stannous chloride solution: First prepare a large amount of sodium chloride solution (2.4%), stored in a plastic bucket for use Stannous chloride 2g was weighed on the shift, and hydrochloric acid (1+1) 5ml was added. The solution was heated at low temperature until it was completely dissolved, and diluted with sodium fluoride solution (2.4%) to 1000 ml.
Second, the analysis operation: Weigh the sample 50mg, placed in a 250ml high beaker, add nitric acid (1 +2.5) 10ml, heated to the sample solution, drop potassium permanganate solution (5%) 6 drops, to Steady purplish red, boiled until brown manganese dioxide precipitated out. Immediately add ammonium molybdate-potassium sodium tartrate solution 10ml, shake, add sodium fluoride-stannous chloride solution 40ml, shake. In a 660nm, 2cm cuvette, water was used as a reference to measure the absorbance.
First, the main reagent
1, nitric acid - silver nitrate (0.4%): In (1 + 4) diluted nitric acid 1000ml, add 4g of silver nitrate; 2, ammonium persulfate solution (15%);
Second, the analysis operation: Weigh 40mg in a 250ml high beaker, add 10ml of nitric acid - silver nitrate solution, heated to dissolve, add 5ml of ammonium persulfate solution, boil 10S, remove, add 40ml, shake, at a wavelength of 530nm Place, 2cm cuvette, water reference, measure the absorbance. Determination of silicon (ferrous reduction - silicon molybdenum blue photometric): First, the main reagent 1, nitric acid (1 +4); 2, potassium permanganate solution (5%); 3, alkaline ammonium molybdate solution: said Take 5g of ammonium molybdate, add 12.5g of potassium carbonate, dissolve, dilute to 100ml; 4, oxalic acid solution (2.5%) 5, ferrous ammonium sulfate solution (1%): Add 1ml of concentrated sulfuric acid per 100ml of solution.
Second, the analysis operation: Weigh the sample 30mg in a 250ml high beaker, add nitric acid (1 +4) 10ml, heated to the sample dissolved, shake the yellow gas away, add 3 drops of potassium permanganate solution, heated to Boiling, remove, immediately add 10ml alkaline ammonium molybdate solution, shake 10 seconds, add 40ml oxalic acid solution, 40ml ferrous ammonium sulfate solution, shake, at a wavelength of 660nm, 0.5cm cuvette, water reference, Measure absorbance. Determination of Phosphorus (sodium fluoride - stannous chloride - Phosphomolybdenum blue photometric method): 1. Main reagent 1, nitric acid (1+2.5); 2, potassium permanganate solution (5%); 3, ammonium molybdate (10%) - Potassium sodium tartrate (10%) (1+1 mixed on the same day); 4, sodium fluoride - stannous chloride solution: First prepare a large amount of sodium chloride solution (2.4%), stored in a plastic bucket for use Stannous chloride 2g was weighed on the shift, and hydrochloric acid (1+1) 5ml was added. The solution was heated at low temperature until it was completely dissolved, and diluted with sodium fluoride solution (2.4%) to 1000 ml.
Second, the analysis operation: Weigh the sample 50mg, placed in a 250ml high beaker, add nitric acid (1 +2.5) 10ml, heated to the sample solution, drop potassium permanganate solution (5%) 6 drops, to Steady purplish red, boiled until brown manganese dioxide precipitated out. Immediately add ammonium molybdate-potassium sodium tartrate solution 10ml, shake, add sodium fluoride-stannous chloride solution 40ml, shake. In a 660nm, 2cm cuvette, water was used as a reference to measure the absorbance.
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