CN1904589A - Technology of photometry determining silicone content in common steel low alloy steel - Google Patents

Abstract

The invention discloses a technology to test the silicon quality in common steel and low alloy steel by photometric method. It includes the following steps: decomposing the tested sample by nitric acid solution, taking oxidation treatment by ammonium persulphate, forming silicon-molybdenum heteropoly acid, using ammonium ferrous sulfate to reduce heteropoly acid to silicon-molybdenum blue and testing the extinction value. The invention could effectively avoid the polymerization of single element silica to make the standard solution could be repeatedly used for several times in certain time range, and the test value would be constant. It has the advantages of good repeatability, high accuracy, low cost, etc.

Description

The technology of silicon amount in the spectrphotometric method for measuring ordinary steel low alloy steel

Technical field

The present invention relates to the technology of silicon amount in the new technology of silicon amount in a kind of spectrphotometric method for measuring iron and steel, particularly spectrphotometric method for measuring ordinary steel low alloy steel.

Background technology

At present, silicon amount in the spectrphotometric method for measuring iron and steel, to realize by standard model, and spectrphotometric method for measuring silicon amount is to be based upon the amount of measuring unimolecule silicic acid in the solution, steel sample is after diluted acid decomposes, reoxidize processing, make its silicon all be oxidized to unimolecule silicic acid, color development is measured under the certain acidity condition.The remaining standard solution in test back must be acid, because unimolecule silicic acid is extremely unstable in acid solution, easily aggregates into polymolecular silicic acid within a certain period of time, as remakes usefulness, and measurement result is passed more and more low in time, generally outwells as waste liquid.

Summary of the invention

Purpose of the present invention promptly is to overcome the shortcoming of prior art, provide a kind of its measurement result that good reappearance is arranged, and the technology of silicon amount in the spectrphotometric method for measuring ordinary steel low alloy steel of higher accuracy and precision, this process using is hanged down acidity solution, reducing the concentration of silicic acid implements to preserve, can effectively prevent the polymerization of unimolecule silicic acid, standard solution is used in the certain hour scope at any time once more even repeatedly, it detects numerical value and remains unchanged.

Purpose of the present invention is achieved through the following technical solutions: the technology of silicon amount in the spectrphotometric method for measuring ordinary steel low alloy steel, and it may further comprise the steps:

(1) gets the standard model of 7 different silicon-containing amounts, take by weighing 0.5g respectively in 7 100ml iron and steel measuring bottles of correspondence, add (1+3) salpeter solution 25ml respectively, after low-temperature heat is decomposed, add 15% ammonium persulfate solution 10ml, continue to boil to solution and emit air pocket, take off, flowing water is cooled to room temperature, is diluted to scale with water, shakes up standby;

(2) pipette above-mentioned standard solution 3.0ml respectively in 5 groups of 100ml conical flasks, each adds mixed acid solution 30ml, shakes up;

(3) get one group of 7 various criterion solution and add 5% ammonium molybdate solution 5ml respectively, shake up, placed 12～15 minutes or boiling water bath 30 seconds, add 5% oxalic acid solution 10ml again, shake up, add 6% l ferrous ammonium sulfate solution 5ml at once, shake up;

(4) at wavelength 670mm place, with 0.5～2.0cm cuvette, be blank with reference to measuring its light absorption value, last with water, draw typical curve or directly adopt average numerical value to calculate, obtain silicon and measure definite value.

The technology of silicon amount in the spectrphotometric method for measuring ordinary steel low alloy steel of the present invention, adopt low acidity solution, reducing the concentration of silicic acid implements to preserve, can effectively prevent the polymerization of unimolecule silicic acid, standard solution is used in the certain hour scope at any time once more even repeatedly, it detects numerical value and remains unchanged, the measurement result reappearance is good, accuracy and precision height, measuring solution can repeatedly use, and saves analysis time effectively, reduces experimentation cost.

Embodiment

The technology of silicon amount in the spectrphotometric method for measuring ordinary steel low alloy steel, it may further comprise the steps:

(1) gets the standard model of 7 different silicon-containing amounts, take by weighing 0.5g respectively in 7 100ml iron and steel measuring bottles of correspondence, add (1+3) salpeter solution 25ml respectively, after low-temperature heat is decomposed, add 15% ammonium persulfate solution 10ml, continue to boil to solution and emit air pocket, take off, flowing water is cooled to room temperature, is diluted to scale with water, shakes up standby;

(2) pipette above-mentioned standard solution 3.0ml respectively in 5 groups of 100ml conical flasks, each adds mixed acid solution 30ml, shakes up;

(3) get one group of 7 various criterion solution and add 5% ammonium molybdate solution 5ml respectively, shake up, placed 12～15 minutes or boiling water bath 30 seconds, add 5% oxalic acid solution 10ml again, shake up, add 6% l ferrous ammonium sulfate solution 5ml at once, shake up;

(4) at wavelength 670mm place, with 0.5～2.0cm cuvette, be blank with reference to measuring its light absorption value, last with water, draw typical curve or directly adopt average numerical value to calculate, obtain silicon and measure definite value.

For the standard test solution of preparing in the technology of verifying silicon amount in the spectrphotometric method for measuring ordinary steel low alloy steel of the present invention can use in the certain hour scope at any time once more even repeatedly, (3), (4) identical method are measured one group respectively on the same day set by step weekly, and calculate the silicon value, following table is the silicon value measured respectively through ten weeks and the standard value result of standard model: the standard value of silicon value and standard model is contrast table as a result:

As can be seen from the above table, the present invention uses same mensuration solution testing after ten weeks, and test data is stable, and measurement result has good reappearance, and higher accuracy and precision, meets the requirement of GB223-89 permissible variation.

Claims (1)

1, the technology of silicon amount in the spectrphotometric method for measuring ordinary steel low alloy steel is characterized in that it may further comprise the steps:

(1) gets the standard model of 7 different silicon-containing amounts, take by weighing 0.5g respectively in 7 100ml iron and steel measuring bottles of correspondence, add (1+3) salpeter solution 25ml respectively, after low-temperature heat is decomposed, add 15% ammonium persulfate solution 10ml, continue to boil to solution and emit air pocket, take off, flowing water is cooled to room temperature, is diluted to scale with water, shakes up standby;

(2) pipette above-mentioned standard solution 3.0ml respectively in 5 groups of 100ml conical flasks, each adds mixed acid solution 30ml, shakes up;

(3) get one group of 7 various criterion solution and add 5% ammonium molybdate solution 5ml respectively, shake up, placed 12～15 minutes or boiling water bath 30 seconds, add 5% oxalic acid solution 10ml again, shake up, add 6% l ferrous ammonium sulfate solution 5ml at once, shake up;

(4) at wavelength 670mm place, with 0.5～2.0cm cuvette, be blank with reference to measuring its light absorption value with water, draw typical curve or directly adopt average numerical value to calculate, obtain silicon and measure definite value.