JPH05157697A - Quantitative analysis of alloy for zirconium - Google Patents

Abstract

PURPOSE:To obtain an ICP method by which a Cu-Cr-Zr alloy can be quantitatively analyzed for zirconium in order to quantitatively recognize the relation between the compounded composition and characteristics of the Cu-Cr-Zr alloy. CONSTITUTION:In the title quantitative analysis, a cutting-dust sample of an alloy is thermally dissolved in aqua regia after the sample is degreased and dried and the dissolved solution is filtrated after cooling. The ash of the filter paper is thermally dissolved in a flux of soda peroxide and sodium carbonate and the flux is thermally dissolved in hydrochloric acid. The filtration of the dissolved solution is obtained. Then the mixed solution of both filtrates is obtained. Ion-exchanged water is added to the mixed solution until a fixed amount is obtained after strontium is added to the mixed solution as a standard reference material and, by using the solution thus prepared as a sample solution, the luminance intensity of the zirconium contained in the alloy is measured by using an inductively coupled plasma method. Then the zirconium content of the alloy is determined by an internal standard method.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for quantitative analysis of zirconium in an alloy by a high frequency inductively coupled plasma emission method (hereinafter referred to as ICP method), particularly in a Cu-Cr-Zr alloy.

[0002]

2. Description of the Related Art A high-speed rotary generator is a gas turbine that burns gas to turn a generator to generate electricity. The heat generated at this time heats hot water to 90% of the original amount of energy.
It is intended to increase the efficiency of%.

When this high-speed rotary generator is used, the conventional 600 rpm is rotated at a high speed of 30,000 rpm, so that centrifugal force is also considerably applied, and it is impossible to use conventional materials in terms of strength. For this reason, miniaturization is being considered in consideration of safety in terms of rotational speed and centrifugal force. In addition, since the rotation speed becomes faster, the temperature also rises to about 350 ° C as compared to 180 ° C in the related art. Therefore, high strength at high temperature is required.

Copper used in rotor bar materials is 200
The strength is only up to ℃, at 350 ℃ is only about half the room temperature. Therefore, we decided to increase the strength by using an alloy of Cr and Zr, and requested the manufacture by an external manufacturer. However, since this is a custom order, it is outside the JIS standard. Therefore, it is necessary to clearly and quantitatively grasp the relationship between the alloy composition and the properties of Cu-Cr-Zr to improve the quality control and process control of the alloy. Therefore, it is indispensable to establish a method for analyzing trace Zr. ..

[0005]

The present invention was devised in view of such problems, and provides an ICP method for quantifying zirconium in an alloy with high sensitivity.

[0006]

[Means for Solving the Problems] That is, the method for quantitatively analyzing zirconium in an alloy according to the present invention comprises degreasing and drying a swarf-like alloy, heating and decomposing it with aqua regia, followed by cooling and decomposing. The filtrate obtained by filtering the liquid and the filter paper is ashed and melted with a flux of sodium peroxide: sodium carbonate, hydrochloric acid is added and dissolved by heating, and then a mixed liquid with the filtered filtrate is prepared. After adding strontium as a standard substance to the mixed solution, make a fixed amount with ion-exchanged water, use this as a sample solution, measure the emission intensity of zirconium using the high frequency inductively coupled plasma emission method, and quantify zirconium by the internal standard method. That is the solution.

[0007]

According to such a quantitative analysis method, a cutting powder-like alloy is thermally decomposed with aqua regia, and a filtrate obtained by filtration,
The filter paper was ashed and melted with a flux of sodium peroxide: sodium carbonate, and the mixture was heated and dissolved by adding hydrochloric acid, and then a mixed solution with the filtered filtrate was prepared. It requires less inspection and can decompose zirconium almost completely.

When the luminescence intensity of zirconium in the sample solution was measured by the ICP method and quantified by the internal standard method, aqua regia, the reagent and the flux had a negative effect. Make the reagent concentration in the sample solution the same,
The influence of the presence of reagents and flux can be suppressed.

Furthermore, both the coefficient of variation and the recovery rate when the synthetic solution was measured were sufficiently satisfactory in practical use, and as a result, zirconium in the alloy was quantified with high sensitivity. A method for the analysis of zirconium has been established to clarify the relationship between alloy composition and properties.

[0010]

EXAMPLES Specific examples of the method for analyzing Zr in the Cu—Cr—Zr alloy according to the present invention will be described below.

First, the basic operation procedure of this embodiment will be described with reference to the flowchart of FIG.

First, in step 101, a sample of powdery Cu-Cr-Zr alloy is degreased with chloroform and dried well, then in step 102 aqua regia is added in a conical beaker, and then in step 103 a predetermined temperature is applied. Heat to decompose. In order to carry out the analysis with higher accuracy, it is preferable to measure the reagents used with a whole pipette, a micropipette or the like.

Next, after cooling this decomposition liquid, step 10
NO in 4. Filter using 5C filter paper and receive in a 200 ml volumetric flask. Next, in step 105, the filter paper and the inner wall of the conical beaker are washed with hydrochloric acid (1 + 5), 2.0 g of strontium is added to the above filtrate, and 200 ml of hydrochloric acid (1 + 5) is added to make a fixed amount. Step 104
The filter paper of No. 1 moves to step 106 and is ashed by a reducing flame of low heat in the Zr crucible, and then in step 107, a flux of sodium peroxide: sodium carbonate (Na ₂ O ₂ : Na ₂ CO ₃ = 2: 1) 2 g
It was thawed in step 108, 40 ml of hydrochloric acid (1 + 1) was added in step 108 to dissolve by heating, and in step 109 NO. Filter using 5C filter paper and add to the filtrate of step 105. Next, in step 110, 2 g of strontium was added to the filtrate as a standard substance.
Then, ion-exchanged water is added to make a fixed amount, and this is used as a sample solution in step 111 in the quantitative analysis method of zirconium in the electrode by the ICP method.

Cu-based on the ICP method according to the present invention will be described below.
Details of the quantitative analysis method of zirconium in the Cr-Zr alloy will be described based on Examples.

[1] Operating procedure of analysis method [1-1 Method of decomposing sample and preparing sample solution] Cu-Cr-Zr alloy that has been cut into chips is degreased with chloroform and dried to obtain a sample. Decomposition was carried out by three methods: solution method, hydrochloric acid-pressure decomposition method, nitric acid-pressure decomposition method, and the residue after decomposition was examined. In addition, 1 part was used for the blank test.

(1) Method of decomposing aqua regia
1 is added and the mixture is decomposed by heating using a burner. After cooling down, N
Filter with o5C filter paper.

(2) Hydrochloric acid-pressure decomposition method and nitric acid-pressure decomposition method A sample of 0.5 g was sampled in a pressure crucible, and a rotor, hydrochloric acid or nitric acid (20 ml) and hydrofluoric acid (0.5 ml) were put in the crucible and sealed. 1
After heating in a constant temperature bath at 70 ° C. for about 1 hour, it is taken out of the constant temperature bath and stirred on a stirrer for 30 minutes. This operation is repeated twice to completely decompose the sample.

After cooling, the total amount of the decomposed liquid was adjusted to 1.00 with boric acid.
Transfer to a poly beaker containing g using ion-exchanged water and heat on a water bath to dissolve boric acid.

After cooling, no. Filter with 5C filter paper and receive the filtrate in a 200 ml volumetric flask.

The filter paper was thoroughly washed with 50 ml of nitric acid and ion-exchanged water, and 2.0 mg of strontium as a standard substance was added to 200 ml by adding to the combined solution of the above filtrate and washing solution.
Use as a sample solution.

(3) Blank 0.5 g of the sample was filtered through a No. 5C filter paper.

[2] Analyzing device, measurement conditions and reagents [2-1 Analyzing device] ICP emission spectroscopic device is IC manufactured by Shimadzu
PS-1000-2 type was used.

[2-2 Measurement Conditions] Table 1 shows the measurement conditions.

[0024]

[Table 1]

[2-3 Reagents] Table 2 shows a list of reagents used in the experiment.

[0026]

[Table 2]

[2-4 Measurement Method] The peak search internal standard method was used.

[3] Result of Decomposition Test FIG. 2 is a graph showing the residue of the sample used in the blank test,
FIG. 3 is a graph showing the residue of the sample subjected to the aqua regia decomposition method. According to the aqua regia decomposition method, it was observed that Cr and a small amount of Zr remained. It is considered that Zr was adsorbed on the filter paper due to insufficient washing.

FIGS. 4 and 5 are graphs showing the residuals after decomposition by the hydrochloric acid-pressure decomposition method and the nitric acid-pressure decomposition method, respectively. Zr was completely decomposed by both decomposition methods.
Some Cu and Cr remained. A large amount of Cr remained in the nitric acid-pressure decomposition method, and a large amount of Cu remained in the hydrochloric acid-pressure decomposition method. The decomposition operability was better in the hydrochloric acid-pressure decomposition method.

It is necessary to melt the residual Cu and Cr, and it is judged that the hydrochloric acid-pressure decomposition method is better in view of operability.

Then, as a countermeasure of the aqua regia decomposition method of (1),
The decomposition residue was examined by performing a 50 ml hydrochloric acid (1 + 5) -water washing method or a hydrochloric acid (1 + 5) washing method. Further, since Zr is considered to be decomposed by nitric acid, a method of decomposing it with nitric acid (1 + 1) and washing the residue with nitric acid (1 + 5) was also performed.

Next, the results of applying the following six decomposition methods to the Cu-Cr-Zr alloy will be described.

[Method a] 0.5 g of a sample is sampled in a conical beaker, and 40 ml of nitric acid (1 + 1) is added to decompose it by heating. After cooling, NO. It was filtered using a 5C filter paper, and the filter paper was washed with 50 ml of nitric acid (1 + 5) and water. As a result, as shown in FIG. 6, the residual amount of Cr is larger than the residual amount of Zr, and Zr is not completely decomposed, which is considered to be inappropriate.

[Method b] 0.5 g of a sample is sampled in a conical beaker, and 40 ml of nitric acid (1 + 1) is added to decompose it by heating. After cooling, NO. After filtering using a 5C filter paper, the filter paper was washed with nitric acid (1 + 5), and the filtrate was adjusted to a fixed amount of 200 ml, and then the acid of the filter paper was washed with water. As a result, as shown in FIG. 7, the residual amount of Cr is larger than the residual amount of Zr, and Zr is not completely decomposed, which is considered to be inappropriate.

[Method c] 0.5 g of a sample is sampled in a conical beaker, and 40 ml of aqua regia is added to decompose it by heating. After cooling, NO. Filter with a 5C filter paper, and filter the filter paper with hydrochloric acid (1
+5) Washed with 50 ml and water. As a result, as shown in FIG. 8, although there is a small amount of Cr residue, Zr is almost decomposed, so it is considered to be appropriate.

[Method d] 0.5 g of a sample is collected in a conical beaker, and 40 ml of aqua regia is added to decompose it by heating. After cooling, NO. Filter with a 5C filter paper, and filter the filter paper with hydrochloric acid (1
+5), and after making the filtrate a fixed amount of 200 ml,
The acid on the filter paper was washed with water. As a result, as shown in FIG. 9, the residual amount of Cr was smaller than that of the method c (FIG. 8), and
It is considered appropriate because r is almost decomposed.

[Method e] 0.5 g of a sample is sampled in a conical beaker, and 40 ml of aqua regia is added to decompose by heating. After cooling, NO. Filter with a 5C filter paper and filter the filter paper with nitric acid (1
+5) Washed with 50 ml and water. As a result, as shown in FIG. 10, the residual amount of Cr is larger than that in the case of the method c (FIG. 8), and therefore it is considered to be inappropriate.

[Method f] 0.5 g of a sample is collected in a conical beaker, and 40 ml of aqua regia is added to decompose it by heating. After cooling, NO. Filter with a 5C filter paper and filter the filter paper with nitric acid (1
+5), and after making the filtrate a fixed amount of 200 ml,
The acid on the filter paper was washed with water. As a result, as shown in FIG. 11, the residual amount of Cr is larger than that in the case of the method e (FIG. 10), and thus it is considered to be inappropriate.

From the above results, it was judged that [Method d] was the most suitable as the decomposition method for the Cu-Cr-Zr alloy.

Therefore, after cooling the decomposition liquid decomposed by the above [Method d], NO. Filter using 5C filter paper, receive in a 200 ml volumetric flask, wash the filter paper and the inner wall of the conical beaker with hydrochloric acid (1 + 5), combine with the previous filtrate, add 2.0 g of strontium, and add hydrochloric acid (1 + 5) To a fixed amount of 200 ml. Furthermore, the filter paper is Z
After ashing with a low flame in a crucible, melt with 2 g of flux of sodium peroxide: sodium carbonate (Na ₂ O ₂ : Na ₂ CO ₃ = 2: 1) and add 40 ml of hydrochloric acid (1 + 1). In addition, it is heated and dissolved, and NO. Filter using 5C filter paper and add to the filtrate.

2 g of strontium as a standard substance was added to this filtrate, and ion-exchanged water was added to make a fixed amount, which was used as a sample solution in the method for quantitative analysis of zirconium in electrodes by the ICP method.

[4] Experiments and Results [4-1 Selection of Analysis Line] In order to select the most suitable wavelength for zirconium analysis, a single solution of each element constituting the Cu—Cr—Zr alloy and an internal standard substance were used. The analytical line was qualitatively selected by using strontium. The results are shown in FIGS.

The concentration of each element in the sample solution was 2 for Cu.
500ppm, Cr 30.0ppm, Zr 10.0
ppm and Sr are 10.0 ppm. Then, three wavelengths having high emission intensity of zirconium were selected and an analysis line was selected.

FIG. 12 shows an emission spectrum of a wavelength of 343.823 nm, FIG. 13 shows an emission spectrum of a wavelength of 339.198 nm, and FIG. 14 shows an emission spectrum of a wavelength of 349.621 nm. It is presumed that it is on the line and does not interfere with zirconium.

Therefore, as the analysis line, 343.823 nm, which has the highest sensitivity in the priority order of the wavelength of zirconium, is adopted.

[4-2 Selection of Sensitivity (HV)] Sensitivity (H
V) is a high voltage applied to Photomal, and an optimum HV exists depending on the concentration.

Therefore, the optimum HV was selected using a 10 ppm zirconium solution. Figure 15 shows the result.
~ Shown in FIG.

FIG. 17 shows the case where the HV is 50,
The emission intensity is saturated. Since the sensitivity HV is preferably as high as possible as long as it is not saturated, here, 40 is adopted as the HV from the results shown in FIG.

[4-3 Selection of Internal Standard Material and Its Wavelength] Strontium is adopted as the internal standard material, and in order to select the analysis line of this strontium, three typical wavelengths of strontium (216.5596 nm, 407. 7
71 nm, 421.522 nm) profile was measured and qualitatively determined. The results are shown in FIGS. 18 to 20 are emission spectra of each element and strontium in the sample after aqua regia decomposition.
Wavelength of 407.771 nm and wavelength of 421.552
In nm, only the emission line of strontium was present and all coexisting substances were on the baseline, and no interference with strontium was observed. The wavelength 216.5596n shown in FIG.
In m, an increase in background (BG) due to the proximity of the emission line of Cu, which is the main component of the coexisting substance, was observed, which is unsuitable as an analysis line.

21 to 23 are emission spectra of each element and strontium when the aqua regia decomposition residue is melted with a fluxing agent. Each wavelength of strontium is 407.771 nm, 4
At 21.552 nm and 216.5596 nm, all coexisting substances were on the baseline and no interference with strontium was observed. From this, the wavelength of 4
07.771 nm and 421.552 nm can be used, but here, as the analysis line, the wavelength 40 with high emission intensity is used.
7.771 nm was adopted.

[4-4 Accuracy of Calibration Curve] The zirconium concentration in the sample solution is about 7 ppm. Therefore, the accuracy of the calibration curve was confirmed in the zirconium concentration range of 0 to 10 ppm. The result is shown in FIG. From this figure, the calibration curve passes almost the origin and the correlation coefficient is 0.99999585.
5, the standard deviation is 0.3462237 ppm, which shows that the accuracy is very good.

[Influence of 4-5 Reagent] Aqua regia was added stepwise to a 7 ppm zirconium solution to quantitatively investigate the influence. The result is shown in FIG.

The determination of the presence or absence of influence is made by the collection rate (measured value x 1
00 / prepared value) ± 2%, and the allowable range is shown by a broken line in the figure.

When measured by the calibration curve method, aqua regia showed a negative effect. This is because the presence of aqua regia increased the viscosity of the sample solution, decreased the amount of sample taken in, and lowered the apparent emission intensity.

Therefore, the concentration of the reagent in the solution for preparing the calibration curve and the concentration of the reagent in the sample solution for analysis were set to be the same to suppress the influence of the presence of aqua regia.

[4-6 Effects of Coexisting Elements] Cu, Cr, and Sr as an internal standard substance were added stepwise to a 10 ppm zirconium solution to quantitatively investigate the effects of these coexisting elements.

The results are shown in FIGS. The determination as to whether or not these effects were exerted was within ± 2% of the recovery rate of zirconium, and is shown by a broken line as an allowable range in the figure. FIG. 26
28. From FIG. 28, it was found that Cu, Cr, and Sr did not affect any of the elements within the allowable range shown by the broken line.

[4-7 Effects of Reagents on Strontium Internal Standard Material] Reagents were added stepwise to a 10 ppm strontium solution to quantitatively investigate the effects. The result is shown in FIG.

As a result, hydrochloric acid and a flux (Na ₂ O ₂ : Na ₂
It was found that both CO ₃ = 2: 1) have a negative effect. That is, as the amounts of hydrochloric acid and flux added increased, the recovery rate of strontium decreased. This is because the coexistence of these reagents increases the viscosity of the sample solution, reduces the amount of sample taken in, and reduces the emission intensity. Therefore, the concentration of the reagent in the solution for preparing the calibration curve and the concentration of the reagent in the analytical test solution were made the same to suppress the negative influence.

[4-8 Effect of Coexisting Element on Internal Standard Material] Cu and C were added to a solution containing 10 ppm of strontium.
The effects of each element on strontium were quantitatively investigated by adding r and Zr in stages. The results are shown in FIGS.

All the elements were within the allowable range shown by the broken line and had no effect on strontium.

[4-9 Verification of Analytical Accuracy Using Synthetic Solution] In order to verify the analytical accuracy under the conditions examined above, a synthetic solution was prepared and implemented. As a result, the recovery rate of zirconium was 99.91% and the coefficient of variation was 1.61%, which was a sufficient accuracy for practical use.

The composition of the synthetic solution is shown in Table 3 and the measurement results are shown in Table 4.

[0064]

[Table 3]

[0065]

[Table 4]

In Table 3, Cu was used by dissolving a metal in nitric acid, and Cr, Zr, and Sr were standard reagents for atomic absorption spectrometry. The solution for preparing the calibration curve was prepared as shown below.

That is, hydrochloric acid 2 was added to a 100 ml volumetric flask.
5 ml, 5 ml of nitric acid and 1.0 mg of strontium were added, and 0 to 1 mg of zirconium was added stepwise, and the amount was made constant with ion-exchanged water.

[5] Consideration From the above results, Cu- by the ICP method according to this example was
The following findings were obtained by examining the analysis method of zirconium in Cr-Zr alloy.

(5-1) Sample Decomposition Method Conventionally, complete decomposition was not possible by dissolving a chipped sample with aqua regia, ashing the residue together with filter paper and melting with a flux. Zirconium can be easily decomposed.

(5-2) Analysis line As a result of examining the interference of coexisting elements at the analysis line 343.823 nm with high emission intensity, no interference peak was observed.

(5-3) Influence and suppression of decomposition reagent The decomposition reagent aqua regia showed negative interference. It is considered that this is because the viscosity of the sample solution increased due to the coexistence of aqua regia and the suction amount of the sample decreased, so in order to suppress this effect, the reagent concentration in the sample solution and the calibration curve preparation solution should be the same. In addition, it was possible to suppress the above-mentioned influence by further measuring by using the strontium internal standard method.

(5-4) Analytical accuracy The recovery rate when measuring 5 synthetic solutions was 99.91%, and the coefficient of variation was 1.61, which were all sufficiently satisfactory for practical use.

[0073]

EFFECT OF THE INVENTION Cu-Cr by the ICP method according to the present invention
According to the method for analyzing zirconium in a Zr alloy, the powdery alloy is thermally decomposed with aqua regia, so that the residual amount of other coexisting substances in the sample solution is small and zirconium is almost decomposed.

When the emission intensity of zirconium in the sample solution was measured by the ICP method and quantified by the calibration curve method,
Although aqua regia, reagents and fluxes have negative effects, it is possible to suppress the effects of the presence of aqua regia, reagents and fluxes by making the reagent concentrations in the calibration curve preparation solution and sample solution the same. It was Further, both the coefficient of variation and the recovery rate when the sample solution was measured by the ICP method were sufficiently satisfactory in practical use, and as a result, a method for analyzing a trace amount of Zr in Cu-Cr-Zr was established. In addition to clarifying the relationship between alloy composition and characteristics, it is possible to improve the quality control and process control of the alloy.

[Brief description of drawings]

FIG. 1 is a flowchart showing a basic operation procedure of a method for quantitatively analyzing zirconium in an alloy according to the present invention.

FIG. 2 is a graph showing a residue of a sample used in a blank test.

FIG. 3 is a graph showing the residue of the sample subjected to the aqua regia decomposition method.

FIG. 4 is a graph showing the residue of a sample after decomposition by a hydrochloric acid-pressure decomposition method.

FIG. 5 is a graph showing the residue of the sample after decomposition by nitric acid-pressure decomposition method.

FIG. 6 is a graph showing the residue of the sample after being decomposed by [Method a] in the detailed description.

FIG. 7 is a graph showing the residue of the sample after being decomposed by [Method b] in the detailed description.

FIG. 8 is a graph showing the residue of the sample after being decomposed by [Method c] in the detailed description.

FIG. 9 is a graph showing the residue of the sample after being decomposed by [Method d] in the detailed description.

FIG. 10 is a graph showing the residue of the sample after being decomposed by [Method e] in the detailed description.

FIG. 11 is a graph showing the residue of the sample after being decomposed by [Method f] in the detailed description.

FIG. 12 is a graph showing emission spectra of various elements at a wavelength of 343.823 nm.

13 is a graph showing emission spectra of various elements at a wavelength of 339.198 nm.

FIG. 14 is a graph showing emission spectra of various elements at a wavelength of 349.621 nm.

FIG. 15: Selection of HV using a solution having a wavelength of 343.823 nm and a zirconium concentration of 10 ppm (in the case of HV30)
The graph that was done.

FIG. 16: Selection of HV using a solution having a wavelength of 343.823 nm and a zirconium concentration of 10 ppm (in the case of HV40)
The graph that was done.

FIG. 17: Selection of HV using a solution having a wavelength of 343.823 nm and a zirconium concentration of 10 ppm (in the case of HV50)
The graph that was done.

FIG. 18 is a graph showing the profile of coexisting substances at a wavelength of 407.771 nm of strontium as an internal standard substance and each element in the sample after aqua regia decomposition.

FIG. 19 is a graph showing profiles of coexisting substances at a wavelength of 421.552 nm of strontium as an internal standard substance and each element in the sample after decomposition of aqua regia.

FIG. 20 is a graph showing the profile of coexisting substances at a wavelength of 216.5596 nm of each element in the sample after aqua regia decomposition and strontium as an internal standard substance.

FIG. 21: Wavelength of each element and strontium 407.7 as an internal standard substance when the aqua regia decomposition residue was melted with a fluxing agent
The graph which shows the profile of a coexisting substance in 71 nm.

FIG. 22: Wavelength 421.5 of each element and strontium as an internal standard when the aqua regia decomposition residue was melted with a fluxing agent
The graph which shows the profile of a coexisting substance in 52 nm.

FIG. 23: Wavelength 216.5 of each element and strontium as an internal standard substance when the aqua regia decomposition residue was melted with a fluxing agent
The graph which shows the profile of a coexisting substance in 96 nm.

FIG. 24 is a graph showing a calibration curve of zirconium.

FIG. 25 is a graph showing the influence of reagents.

FIG. 26 is a graph quantitatively showing the allowable range of the recovery rate of zirconium due to the influence of Cu.

FIG. 27 is a graph quantitatively showing the allowable range of the recovery rate of zirconium due to the influence of Cr.

FIG. 28 is a graph quantitatively showing the allowable range of the recovery rate of zirconium due to the influence of Sr.

FIG. 29 is a graph showing the influence of reagents on strontium.

FIG. 30 is a graph quantitatively showing the allowable range of the recovery rate of strontium due to the influence of Cu.

FIG. 31 is a graph quantitatively showing the allowable range of the recovery rate of strontium due to the influence of Cr.

FIG. 32 is a graph quantitatively showing the allowable range of the strontium recovery rate due to the influence of Zr.

Claims (2)

[Claims] 1. A cutting powdery alloy is degreased and dried, aqua regia is added thereto for thermal decomposition and then cooled, and a filtrate obtained by filtering the decomposed solution and filter paper are ashed to obtain sodium peroxide: Melt with a fluxing agent of sodium carbonate, add hydrochloric acid to dissolve by heating, and then create a mixed solution with the filtered filtrate, add strontium as a standard substance to this mixed solution, and make a fixed amount with ion-exchanged water. A quantitative analysis method of zirconium in an alloy, which comprises measuring the emission intensity of zirconium by using a high frequency inductively coupled plasma emission method as a sample solution and quantifying zirconium by an internal standard method. 2. The method for quantitative analysis of zirconium in an alloy according to claim 1, wherein the sample alloy is a Cu—Cr—Zr system.