CN115127953A - Method for eliminating interference during determination of oxygen content of non-magnetic steel - Google Patents

Abstract

The invention relates to a method for eliminating interference during non-magnetic steel oxygen content measurement, which prepares required reagents, materials, instruments and equipment according to the national standard GB/T11261-2006; processing and polishing the sample according to the national standard, subtracting the end part by using a wire cutter or a shearing machine, and shearing a sample with the mass of 0.1000-0.2000 g; sequentially cleaning the mixture for 3-7 minutes by using carbon tetrachloride or diethyl ether and acetone in an ultrasonic cleaner, drying the mixture by using hot air, and putting the mixture into a dryer for later use; before analysis, checking by using a steel certified standard substance indicating oxygen content, wherein the used real standard oxygen content is greater than the oxygen content of the analyzed sample, the range value between the three times of correction values is less than a repeatability value, and otherwise, correcting again; weighing 0.1000-0.2000 g of a test material by a ten-thousandth analytical balance until the weight is 0.1 mg; the blank test and the measurement are carried out according to the national standard, and the problem that the detection value is continuously reduced during continuous detection due to the interference of the measurement of the oxygen content caused by the overlarge amount of Cr, Mn and Ni alloy elements entering an instrument during the detection can be overcome.

Description

Method for eliminating interference during determination of oxygen content of non-magnetic steel

Technical Field

The invention relates to a method for measuring the oxygen content of a steel material, in particular to a method for eliminating interference during the measurement of the oxygen content of non-magnetic steel, which can overcome the problem that the measured value is continuously reduced during continuous detection because the measured oxygen content is interfered due to the overlarge amount of Cr, Mn and Ni alloy elements entering an instrument during the detection.

Background

The national determination standard of the oxygen content of steel products is 'pulse heating inert gas melting-infrared absorption method GB/T11261-2006', the principle, reagents, materials, instruments, equipment, sampling and sample preparation method and other contents are scientifically specified, most brands of steel products are normally detected according to the standard, but when the oxygen content of non-magnetic steel products is detected, the phenomenon of unstable detection result of oxygen occurs: when the same sample with uniform oxygen content is continuously detected, the detection value continuously decreases and even becomes a negative value. The phenomenon is frequently generated in the same industry detection at present. The national standard is not completely applicable to all steel types, and the non-magnetic steel oxygen content can be accurately measured only by adopting a more scientific method to eliminate interference when detecting non-magnetic steel products.

According to research, the non-magnetic steel products contain high content of alloy elements such as Cr, Mn and Ni, about 0.5-1.0 g of sample is weighed according to the analysis steps of the national standard (GB/T11261-2006), and the amount of the alloy elements such as Cr, Mn and Ni entering an instrument during detection is too large, so that certain interference is formed on the determination of oxygen content, and the alloy elements are easy to remain in the instrument, so that the detection value is continuously reduced during continuous detection. Therefore, it is necessary to reduce the amount of the alloy elements such as Cr, Mn, and Ni entering the apparatus in the analysis step, that is, to reduce the quality of the sample entering the apparatus, and stable and reliable data can be obtained in accordance with the analysis step of the national standard (GB/T11261-2006).

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provide a method for eliminating interference in the measurement of the oxygen content of non-magnetic steel, which can obtain stable and reliable data by reducing the amount of Cr, Mn and Ni alloying element substances entering an instrument, namely reducing the quality of a sample entering the instrument.

The purpose of the invention is realized as follows: a method for eliminating interference during determination of oxygen content of non-magnetic steel sequentially comprises the following steps:

step 1), preparing required reagents, materials, instruments and equipment according to the national standard GB/T11261-2006;

step 2), sample preparation: processing and polishing a sample according to the national standard GB/T11261-2006, subtracting the end part by using a wire cutter or a shearing machine after polishing, and shearing a sample with the required mass of 0.1000-0.2000 g; sequentially cleaning the mixture for 3-7 minutes by using carbon tetrachloride or diethyl ether and acetone in an ultrasonic cleaner, drying the mixture by using hot air, and putting the mixture into a dryer for later use;

step 3), preparing an instrument: before analysis, the instrument is in a normal state, before analysis, a steel certified standard substance indicating the oxygen content is used for checking, the oxygen content of the used physical standard is greater than that of the analyzed sample, the extreme difference value between the three correction values is smaller than the repeatability value, otherwise, the correction is carried out again;

step 4), an analysis step:

4.1) weighing 0.1000-0.2000 g of sample by a ten-thousandth analytical balance to be accurate to 0.1 mg;

4.2) and the rest steps, and performing blank tests and determination according to the national standard (GB/T11261-2006).

The invention has the following positive effects:

when the method of the invention is used for detecting the oxygen content of the non-magnetic steel product, the amount of Cr, Mn, Ni and other alloy elements entering an instrument during detection is reduced, so that the oxygen element is prevented from being absorbed and interfered during the detection process, thereby obtaining continuous and stable data. The following table 1 shows the detection results of the same batch of non-magnetic steel products with uniform oxygen content, and after comparison, the invention has positive effects.

TABLE 1

Detailed Description

According to the research data of the determination of the oxygen content of the non-magnetic steel, the content of the principle, reagents, materials, instruments, equipment and the like of the national standard (GB/T11261-2006) related to the invention does not need to be adjusted; it is the first of the sampling and analysis steps that need to be adjusted.

Preparing a sample: processing and polishing the sample according to the national standard (GB/T11261-2006), subtracting the end part by using a wire cutting pliers or a shearing machine after polishing, and shearing off the sample with the required mass (0.1000-0.2000 g). And (3) sequentially cleaning the glass substrate by using carbon tetrachloride (or diethyl ether) and acetone in an ultrasonic cleaner for 3-7 minutes, carefully drying the glass substrate by using hot air, and then placing the glass substrate into a dryer for later use.

First analysis step: weighing 0.1000-0.2000 g of sample with ten-thousandth analytical balance to 0.1 mg.

Example 1: a method for eliminating interference in determination of oxygen content of non-magnetic steel sequentially comprises the following steps:

step 1), preparing required reagents, materials, instruments and equipment according to the national standard GB/T11261-2006;

step 2), sample preparation: processing and polishing a sample according to the national standard GB/T11261-2006, subtracting an end part by using a wire cutting pliers or a cutting machine after polishing, and cutting off a sample with required mass (0.1000-0.2000 g); and (3) sequentially cleaning the glass substrate by using carbon tetrachloride or diethyl ether and acetone in an ultrasonic cleaner for 3-7 minutes, and carefully drying the glass substrate by using hot air and then placing the glass substrate into a dryer for later use.

Step 3), preparing an instrument: the instrument should be in a normal state before analysis; before analysis, the steel certified standard substance with the oxygen content is used for inspection, the oxygen content of the used physical standard is greater than that of the analyzed sample, the range difference between the three correction values is less than the repeatability value, and otherwise, the correction should be carried out again.

Step 4), an analysis step:

4.1), weighing 0.1000-0.2000 g of sample by a ten-thousandth analytical balance to the accuracy of 0.1 mg.

4.2) and the rest steps, and performing blank tests and determination according to the national standard (GB/T11261-2006).

Claims (1)

1. A method for eliminating interference during determination of oxygen content of non-magnetic steel is characterized by sequentially comprising the following steps:

step 1), preparing required reagents, materials, instruments and equipment according to the national standard GB/T11261-2006;

step 2), sample preparation: processing and polishing a sample according to the national standard GB/T11261-2006, subtracting the end part by using a wire cutter or a shearing machine after polishing, and shearing a sample with the required mass of 0.1000-0.2000 g; sequentially cleaning the mixture for 3-7 minutes by using carbon tetrachloride or diethyl ether and acetone in an ultrasonic cleaner, drying the mixture by using hot air, and putting the mixture into a dryer for later use;

step 3), preparing an instrument: before analysis, the instrument is in a normal state, before analysis, a steel certified standard substance indicating the oxygen content is used for checking, the oxygen content of the used physical standard is greater than that of the analyzed sample, the extreme difference value between the three correction values is smaller than the repeatability value, otherwise, the correction is carried out again;

step 4), an analysis step:

4.1) weighing 0.1000-0.2000 g of sample by a ten-thousandth analytical balance to be accurate to 0.1 mg;

4.2) and the rest steps, and performing blank test and determination according to the national standard (GB/T11261-2006).