CN105277533A - Method for determining content of zirconium in steel - Google Patents

Abstract

The invention discloses a method for determining the content of zirconium in steel. The method is characterized in that a sample is dissolved in an acid, and an inductively coupled plasma spectrometer is adopted to directly determine the content of zirconium in steel, and the detection range is 0.001-0.100%. The above analysis method has the advantages of simplicity, fastness, small amount of reagents used in the invention, fast analysis speed, good precision, and high accuracy, and meets scientific research and production demands. The method comprises the following steps: placing the sample in a polytetrafluoroethylene beaker, adding a hydrochloric acid and nitric acid mixed acid with the volume ratio of hydrochloric acid to nitric acid of 3:1, dissolving the sample, taking down the beaker, slightly cooling, transferring the obtained cooled solution to a volumetric flask, diluting with pure water, shaking up, and carrying out blank test together with the sample; selecting the zirconium analysis spectrum line of 339.197nm on the inductively coupled plasma spectrometer, simultaneously determining the zirconium spectrum intensity of a zirconium work curve standard solution and the sample solution, and automatically regressing through a computer to calculate an analysis result.

Description

The assay method of zirconium content in a kind of steel

Technical field

The present invention relates to metallurgical analysis technical field, particularly relate to the assay method of zirconium content in a kind of steel.

Background technology

In metallurgical industry, zirconium Chang Zuowei deoxygenation sulphur removal and dephosphorization agent.Although the zirconium content in some steel is low, comparatively large on the impact of steel, it can improve intensity and the hardness of steel, improves the welding performance of steel.

In steel, the traditional analysis of zirconium content mainly contains photometry, as tribromo azo chlorine phosphorus Cerium-group REE, to chlorine (bromine) mandelic acid precipitation zirconium---Arsenazo Ⅲ Photometric Method, arsenazo Ⅲ Cerium-group REE.Arsenazo Ⅲ Photometric Method applies maximum analytical approachs, because chromogenic reaction can be carried out in strong acid media, selectivity is very high.But the analysis for trace Zirconium also will do necessary separation and consentration.Its maximum feature needs to eliminate interference element, and analysis process is longer, and agents useful for same is more.

Up to the present, in steel, the analysis of zirconium content detects there are no national standard method and rower method.

Summary of the invention

The technical problem to be solved in the present invention is to provide the assay method of zirconium content in a kind of steel, after the present invention adopts acid dissolve sample, inductively-coupled plasma spectrometer is utilized directly to measure zirconium amount in steel, inspection range is wider is 0.001 ~ 0.100%, analytical approach simple and fast, and agents useful for same is less, analysis speed is fast, precision is good, and accuracy is high, meets the demand of research and production.

For reaching above-mentioned purpose, the assay method of zirconium content in a kind of steel of the present invention, comprises the following steps:

(1) sample is placed in polytetrafluoroethylene beaker, adds the nitration mixture of sal prunella volume ratio 3:1, hydrofluorite, sample dissolution, take off afterwards slightly cold after be transferred in volumetric flask, with pure water dilution, shake up, do blank test in company with sample;

(2) on inductively-coupled plasma spectrometer, select the analysis spectral line 339.197nm of zirconium, to the spectral intensity of zirconium working curve standard solution and test solution Simultaneously test zirconium, computing machine automatic returning calculates analysis result;

Wherein being formulated as of zirconium working curve standard solution:

When in sample during zirconium content≤0.08%, claim 0.2000g high purity iron, undertaken shifting respectively in 6 100mL plastics volumetric flasks after sample dissolves cooling by step (1), add zirconium mark liquid to be respectively mixed with zirconium content and to be: 0%, 0.0050%, 0.010%, 0.025%, 0.050%, 0.100%, the working curve standard solution of 6 points, adding of zirconium amount is respectively: 0mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL, 2.00mL;

As zirconium content > 0.08%, claim high purity iron 0.1000g, undertaken shifting respectively in 6 100mL plastics volumetric flasks after sample dissolves cooling by step (1), add zirconium mark liquid to be respectively mixed with zirconium content and to be: 0%, 0.0050%, 0.010%, 0.025%, 0.050%, 0.100%, the working curve standard solution of 6 points, adding of zirconium amount is respectively 0mL, 0.50mL, 1.00mL, 2.50mL, 5.00mL, 10.00mL.

Wherein said hydrochloric acid density is 1.19, and described nitric acid density is 1.42, and described hydrofluorite density is 1.13.

The invention difference from existing technology is that the present invention achieves following technique effect:

1) decomposition of sample: after steel curved beam sal prunella nitration mixture, hydrofluorite low-temperature heat dissolve, cooling, with water constant volume.Chemical reagent used is less, cost efficiency;

2) on ICP-AES spectrometer, sample directly can be gone up machine and measure after dissolving constant volume.Fast easy and simple to handle;

3) inspection range is wider is 0.0010 ~ 0.100%, analytical approach simple and fast, and agents useful for same is less, and precision is good, and accuracy is high, meets the demand of research and production, has application value.

Embodiment

Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.

1. method summary

After sample sal prunella nitration mixture, hydrofluorite low-temperature heat dissolve, with water constant volume, measure zirconium content in solution by ICP-AES method.

2. prepare analyrical reagent, standard solution, instrument.

2.1 sal prunella nitration mixture (3+1), are prepared in proportion by hydrochloric acid (ρ 1.19, top grade is pure), nitric acid (ρ 1.42, top grade is pure); Hydrofluorite (ρ 1.13, top grade is pure).

2.2 zirconium standard solution: with the zirconium standard solution (national ferrous materials test center Iron and Steel Research Geueral Inst) of 1000 μ g/mL, dilution is mixed with the zirconium standard solution of 100.0 μ g/mL, 10.0 μ g/mL.

2.3 high purity irons (Fe>99.98%)

2.4 experimental waters are secondary pure water

2.5 key instruments and test condition

2.5.1 U.S. PE company produces, Optima5300DV inductively-coupled plasma spectrometer.

2.5.2 instrument parameter: see running parameter table 1

Running parameter table 1

2.5.3 the analysis of line wavelength of zr element adopts 339.197nm.

3. measure

3.1 analytical procedure

Claim 0.1 ~ 0.2g sample, be accurate to 0.0002g, in polytetrafluoroethylene beaker, add 10mL sal prunella nitration mixture, 2mL hydrofluorite, low-temperature heat is dissolved, take off slightly cold after be transferred in 100mL plastics volumetric flask, be diluted to scale with pure water, shake up (doing blank test in company with sample).On inductively-coupled plasma spectrometer, under selected Instrument working parameter (see table 1), by atomizer and the quarter bend system of hydrofluoric acid resistant, select the optimized analysis spectral line 339.197nm of zirconium, to the spectral intensity of zirconium working curve standard solution and test solution Simultaneously test zirconium, computing machine automatic returning calculates analysis result.According to the performance characteristics of different inductively-coupled plasma spectrometers, other glitch-free zirconium analytical lines also can be selected to analyze.

The preparation of 3.2 zirconium working curve standard solution: when in sample during zirconium content≤0.08%, claim 0.2000g high purity iron, undertaken shifting respectively in 6 100mL plastics volumetric flasks after sample dissolves cooling by 3.1 steps, add 10.0 μ g/mL zirconium mark liquid to be respectively mixed with zirconium content and to be: 0%, the working curve standard solution of 0.0050%, 0.010%, 0.025%, 0.050%, 0.100% (finally this point is prepared with the zirconium mark liquid of 100.0 μ g/mL) 6 points, adding of zirconium amount is respectively: 0mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL, 2.00mL; As zirconium content > 0.08%, claim high purity iron 0.1000g, undertaken shifting respectively in 6 100mL plastics volumetric flasks after sample dissolves cooling by 3.1 steps, add 10.0 μ g/mL zirconium mark liquid to be respectively mixed with zirconium content and to be: 0%, the working curve standard solution of 0.0050%, 0.010%, 0.025%, 0.050%, 0.100%6 point, adding of zirconium amount is respectively 0mL, 0.50mL, 1.00mL, 2.50mL, 5.00mL, 10.00mL.

4 preci-sion and accuracy experiments

To three steel standard models, empirically method carries out the test of precision, accuracy.Analysis result is in table 2.

Precision, accuracy test table 2

5 conclusions

As can be seen from Table 2, the inventive method has higher precision and good accuracy, can meet the needs of production and scientific research, have application value.

Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.

Claims (2)

1. the assay method of zirconium content in steel, is characterized in that comprising the following steps:

(1) sample is placed in polytetrafluoroethylene beaker, adds the nitration mixture of sal prunella volume ratio 3:1, hydrofluorite, sample dissolution, take off afterwards slightly cold after be transferred in volumetric flask, with pure water dilution, shake up, do blank test in company with sample;

(2) on inductively-coupled plasma spectrometer, select the analysis spectral line 339.197nm of zirconium, to the spectral intensity of zirconium working curve standard solution and test solution Simultaneously test zirconium, computing machine automatic returning calculates analysis result;

Wherein being formulated as of zirconium working curve standard solution:

When in sample during zirconium content≤0.08%, claim 0.2000g high purity iron, undertaken shifting respectively in 6 100mL plastics volumetric flasks after sample dissolves cooling by step (1), add zirconium mark liquid to be respectively mixed with zirconium content and to be: 0%, 0.0050%, 0.010%, 0.025%, 0.050%, 0.100%, the working curve standard solution of 6 points, adding of zirconium amount is respectively: 0mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL, 2.00mL;

As zirconium content > 0.08%, claim high purity iron 0.1000g, undertaken shifting respectively in 6 100mL plastics volumetric flasks after sample dissolves cooling by step (1), add zirconium mark liquid to be respectively mixed with zirconium content and to be: 0%, 0.0050%, 0.010%, 0.025%, 0.050%, 0.100%, the working curve standard solution of 6 points, adding of zirconium amount is respectively 0mL, 0.50mL, 1.00mL, 2.50mL, 5.00mL, 10.00mL.

2. the assay method of zirconium content in steel according to claim 1, it is characterized in that: described hydrochloric acid density is 1.19, described nitric acid density is 1.42, and described hydrofluorite density is 1.13.