JPH06186221A - Method and apparatus for simultaneously analyzing sulfur and phosphorus in metal sample - Google Patents

Abstract

PURPOSE:To determine the quantities of sulfur and phosphorus in a metal sample quickly at the same time. CONSTITUTION:A metal sample 10 undergoes electrolysis or is made to react with oxygen having reducing power in a hydride-gas generating device 1, and hydride gas of phosphorus and sulfur in the sample is generated. Inactive gas is supplied into the hydride gas generating device 1. The above described hydride gas is introduced into a hydride-gas determining device 12 together with the inactive gas. The carrier gases are brought into contact with or made to pass through H2S detecting test paper or pH3 detecting test paper. The H2S detecting test paper is impregnated with a reagent which chemically reacts with H2S and develops a color. The pH3 detecting test paper is impregnated with a reagent which chemically reacts with pH3 and develops a color. Thus, both test papers are colored. The intensities of the coloring are measured, respectively.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sulfur and phosphorus analysis method and apparatus capable of simultaneously and rapidly determining a minute amount of sulfur and phosphorus contained in a metal sample. INDUSTRIAL APPLICABILITY The present invention is used in the field of manufacturing process control and quality control analysis in the iron manufacturing industry or various non-ferrous metal industries.

[0002]

2. Description of the Related Art In the management of operations such as metal refining and steelmaking processes, it is necessary to analyze and grasp the component content rates as quickly as possible, and to take operational countermeasures according to the results. For example, in the steelmaking process, the time from sampling to obtaining analytical results is usually 5 to 6 minutes. In addition, high accuracy and rapid analysis are required for product verification. Among the components to be analyzed, sulfur and phosphorus are important in determining the quality especially in iron making.

As a method for quantifying a very small amount of sulfur in a metal sample, there is a combustion-infrared absorption method defined in JIS G1215 "Method for quantifying sulfur in iron and steel".
In this method, a metal sample is burned in an oxygen stream to convert sulfur in the sample into sulfur dioxide, and the content rate is obtained from its infrared absorption intensity. Although this analysis method is excellent in quantitative sensitivity, there is a problem in that it takes a long time to perform the analysis including the sample pretreatment for cutting or cutting the sample into small lumps. Further, as a method for quantifying a trace amount of phosphorus, for example, JIS G1214 is used.
There is a molybdenum blue absorptiometric method defined in "Method for determination of phosphorus in iron and steel". This method measures the absorbance of molybdenum blue produced by decomposing a sample with acid, oxidizing phosphorus by white smoke treatment with perchloric acid, and then heating it together with ammonium molybdate to reduce phosphomolybdic acid produced. Is. A major problem with this phosphorus determination method is that the analysis operation is complicated and skill is required.

In order to improve these problems, the inventors of the present invention have proposed that "a method for electrolysis gasification of a metal material and its apparatus" (Japanese Patent Application No. 2-44485) to provide sulfur in a sample,
A new analysis method for phosphorus, carbon, etc. was proposed. In this analysis method, a metal sample is electrolyzed in an electrolytic solution to generate a quantification target component such as sulfur, phosphorus, and carbon as a hydride gas, and a gas chromatograph analysis device, an inductively coupled plasma emission spectroscopic analysis device, and an atomic absorption analysis device are used. Alternatively, the gas component concentration is measured by a gas analyzer such as a visible or ultraviolet absorption spectrophotometer to determine the content of each component in the sample. By using this method, it has become possible to quantify sulfur and phosphorus in metal samples more easily and quickly than in the past, but if the sensitivity of the gas analyzer is not sufficient or the sensitivity is good, both Ppm due to problems such as not being able to quantify elements simultaneously
Simultaneous determination of order sulfur and phosphorus was difficult.

Therefore, the analysis target is limited to only sulfur and phosphorus,
As a highly sensitive and rapid analysis method, "Analysis method of phosphorus and sulfur in metal sample and its apparatus" (Japanese Patent Application No. Hei 3)
-160587) and "Method and apparatus for analysis of trace amounts of phosphorus and sulfur in metal sample" (Japanese Patent Application No. 3-1889).
75) was proposed. In these methods, a test paper photoelectric photometric method (reflection photometric method) that can detect hydride gases of sulfur and phosphorus with high sensitivity is used as a gas analyzer, and electrolysis or reaction with an acid having reducing power is adopted. To generate sulfur and phosphorus in the sample as hydride gas, and detect the concentration of the generated gas to quantify sulfur and phosphorus. This method has made it possible to quantify sulfur and phosphorus up to the ppm order.

[0006]

In recent years, the development of high-purity metals has been actively pursued along with the upsizing of products, and the components contained in the materials have been steadily decreasing. Taking steel products as an example, high-grade steel products in which the content components of sulfur, phosphorus, etc. are controlled in the ppm order have been developed. Therefore, there is an increasing need for accurate analysis of a small amount of contained components, and a rapid analysis is required to utilize the analysis result for manufacturing process control.

The above-mentioned "Method and apparatus for analyzing phosphorus and sulfur in metal sample" (Japanese Patent Application No. 3-160587) and "Method and apparatus for analyzing a trace amount of phosphorus and sulfur in metal sample" (Japanese Patent Application No. 3-539). -188975), it became possible to quantify sulfur and phosphorus in the ppm order by adopting a test paper photoelectric photometric method in a gas analyzer. However, in these methods, since one type of test paper is used to detect hydride gas, only one component of H ₂ S or PH ₃ can be detected, and sulfur and phosphorus can be quantified at the same time. It was difficult. INDUSTRIAL APPLICABILITY The present invention provides an analysis method and an apparatus thereof capable of simultaneously and rapidly determining a small amount of sulfur and phosphorus contained in a metal sample.

[0008]

In order to solve the above problems, the present inventors have found that the following method and apparatus are effective. That is, in a hydride gas generator, a metal sample is reacted with an acid having an electrolyzing or reducing power to generate a hydride gas of sulfur and phosphorus in the sample, while the hydride gas generating the hydride gas is present. In a method for quantifying sulfur and phosphorus in a metal sample by supplying an inert gas into the device and guiding the hydride gas together with the inert gas to a hydride gas quantification device, a gas contact chamber of the hydride gas quantification device. supplying PH ₃ detection test paper impregnated with a reagent that exhibits H ₂ S and the chemical reaction H ₂ S detection test paper impregnated with a reagent that exhibits coloration occurs and results in PH ₃ and a chemical reaction color development, The sulfur and phosphorus in the metal sample are characterized in that the hydride gas is brought into contact with each of the test strips to cause the test strips to develop color, and the color development intensity is measured to simultaneously determine sulfur and phosphorus. In the gas contact chamber of the hydride gas quantification device, the hydride gas is in contact with the H ₂ S detection test strip and then with the PH ₃ detection test strip. And a hydride gas generator for generating H ₂ S and PH ₃ from the metal sample, and the hydride gas is present in order to realize the simultaneous analysis of sulfur and phosphorus in the metal sample. In an analyzer equipped with a device for supplying an inert gas into the hydride gas generator, and a hydride gas quantification device for quantifying the hydride gas introduced together with the inert gas, the hydride gas quantification device is: comprising a PH ₃ detection test paper impregnated with a reagent that exhibits H ₂ S and the chemical reaction H ₂ S detection test paper and impregnated with a reagent that exhibits coloration caused the resulting PH ₃ is a chemical reaction color Further, a gas contacting chamber for contacting both of the test papers and the hydride gas is provided, and monochromatic light is irradiated on the gas contacting surface of each test paper to detect the reflected light intensity and measure the concentration of sulfur and phosphorus. Is a means for using a simultaneous analyzer for sulfur and phosphorus in a metal sample, characterized in that it is provided with a color intensity detector capable of H ₂ S in
After supplying the test paper for detection and passing the whole amount of the carrier gas from one side of the test paper to the opposite side, the whole amount of the carrier gas is changed to PH ₃
Concentrations of sulfur and phosphorus are provided by providing a gas contact chamber with a structure that allows one side of the test strip for detection to pass in the opposite direction, and irradiating monochromatic light on the gas inflow side of each test strip and detecting the reflected light intensity. Means for using a simultaneous analyzer for sulfur and phosphorus in a metal sample, which is equipped with a color development intensity detector capable of measuring, or in the above analyzer,
The hydride gas meter supplies the test paper for PH ₃ detection under the test paper for H ₂ S detection in the gas transportation path, and supplies the total amount of carrier gas from the top surface of the test paper for H ₂ S detection to PH.
₍₃₎ A test chamber for detection is provided with a gas contact chamber that passes in the direction of the lower surface, and after separating each test strip, the gas inflow surface of each test strip is irradiated with monochromatic light to detect its reflected light intensity. It is a means for using a simultaneous analyzer for sulfur and phosphorus in a metal sample, which is equipped with a color development intensity detector capable of measuring the concentrations of sulfur and phosphorus.

[0009]

[Function] When a metal sample is reacted with an acid having electrolysis or reducing power, sulfur and phosphorus in the metal sample are reduced,
H ₂ S and PH ₃ are generated. In the present invention, the metal sample to be analyzed may be either block-shaped or cut-shaped. In the iron-making industry, a cylindrical block-shaped sample having a diameter of about 30 mm, which is sampled from hot metal or molten steel and prepared by a sample preparation device, is often used. Generation of hydride gas from a metal sample is performed in a closed hydride gas generator, and in the case of reacting only with an acid, 30 to 11
Suitable is 3-12M hydrochloric acid heated to 0 ° C. Further, by using hydrochloric acid as an electrolytic solution and installing a counter electrode to electrolyze the sample, the amount of sample dissolved per unit time can be increased and the amount of hydride gas generated can be improved.
The generated hydride gas is conveyed to the hydride gas quantitative device by the inert gas. Argon as the inert gas,
Helium or nitrogen gas is used.

The hydride gas conveyed to the hydride gas meter is continuously supplied to the H ₂ S detection test strip and the PH ₃ detection test strip which continuously or intermittently run in the gas contact chamber. To be done. As the detection test papers, a commercially available reagent having a width of about 2 cm which is impregnated with reagents such as lead acetate and silver nitrate impregnated with a reagent which causes a color reaction by chemically reacting with H ₂ S and PH ₃ , respectively, can be used. The running speed of the test paper is appropriately adjusted according to the amount of gas generated, and 1 to 10 cm / min is suitable for continuous measurement, and 10 to 60 seconds / 1 is suitable for intermittent running.

The method of contacting the transported hydride gas with both test strips is such that one side of each test strip is brought into contact with the carrier gas filled in the gas contact chamber of a constant volume, or from the upper surface to the lower surface of the test strip. Any of the methods of passing the carrier gas may be used. Both test papers can detect the total amount of H ₂ S and PH _{3 in} a trace amount of about 100 ppm or less. When the reagent impregnated in the test paper reacts with the hydride gas, color develops on the surface of the test paper,
The gas concentration can be measured by detecting the color development intensity. Since each test paper develops a color by a specific gas, there are few interfering components at the time of detection. When H ₂ S and PH ₃ coexist, the H ₂ S detecting test strip detects only H ₂ S and does not detect PH ₃ at all. Meanwhile, PH ₃ detection test paper would also detects H ₂ S detects the PH _3.

[0012] Although the detection sensitivity for H ₂ S of PH ₃ detection test strip is less than 1/10 of PH _3, H ₂ S and P
Depending on the H ₃ concentration, it may cause an increase in the error in the quantitative value. Therefore, in order to detect both gas components without interfering with the gas in which H ₂ S and PH ₃ coexist, the gas to be measured was first contacted with or passed through the H ₂ S detection test strip. After that, the test paper for PH ₃ detection may be contacted with or passed through. Trace amount of H ₂ less than 100ppm
S If the total amount is consumed by reacting with reagent impregnated in the H ₂ S detection test paper, that only PH ₃ is present in the gas after contact or pass in H ₂ S detection test paper become. By detecting this gas with a PH ₃ detecting test strip, H ₂ S and PH ₃ can be detected in the state where no interfering component is present. If the high concentration of H ₂ S is at risk of coexisting is a gas after contact or pass in H ₂ S detection test strip is passed through a lead acetate filter H ₂
After completely removing only S, the test sheet for detecting PH ₃ may be brought into contact with or passed through.

In order to measure the color development intensity of the color-developed test paper, the color development part of the gas contact surface or the gas inflow surface of each test paper is irradiated with a single wavelength lamp, and the intensity of the reflected light is measured with a photodiode or the like. taking measurement. Both H ₂ S detection test paper and PH ₃ detection test paper have a color of 55.
It is possible to detect at the same wavelength of about 5 nm. It is possible to perform simultaneous quantification of phosphorus and sulfur based on the reflected light intensity by previously obtaining a calibration curve showing the relationship between the sulfur and phosphorus content and the color development intensity (reflected light intensity) by an experiment.

[0014]

EXAMPLES Examples of the present invention will be described below. FIG. 1 schematically shows an example of a hydride gas generator that generates a hydride gas by electrolysis using a block-shaped steel sample.

The hydride gas generator 1 comprises a reaction chamber 2, and a nitrogen gas cylinder 3 is connected to the upper side surface of the reaction chamber 2 via a needle valve 4 and a flow meter 5. The opening of the needle valve 4 is adjusted to keep the flow rate of nitrogen gas supplied to the reaction chamber 2 constant. Further, a gas-liquid separator 6 is connected to the reaction chamber 2 on the side opposite to the side to which the nitrogen gas cylinder 3 is connected. An electrolyte pump 8 is provided on the lower side surface of the reaction chamber 2.
The electrolytic solution tank 7 is connected via the heat exchanger 9. As the electrolytic solution, various compositions can be used, but 6M HCl was used. The top of the reaction chamber 2 serves as a holder for the block-shaped steel sample, and the sample 10 is supported so that the lower end thereof enters the reaction chamber 2. The top of the gas-liquid separator 6 is connected to the hydride gas metering device 12 via a line filter 11, and the bottom is connected to the electrolyte tank 7.

The hydride gas generator 1 is equipped with an electrolyzer 13, a sample electrode (positive electrode) 14 contacts the upper surface of the sample 10, and a counter electrode (negative electrode; not shown) of the sample 10 in the reaction chamber 2. It is located near the bottom surface. The sample electrode 14 and the counter electrode are connected to a power supply 16, and the power supply 16 is connected to a voltage control circuit 15. A reference electrode (not shown) is inserted between the counter electrode and the lower surface of the sample 10. The reference electrode is connected to the voltage control circuit 15 via the voltage measuring circuit 17. Based on the voltage detected by the reference electrode, the electrolytic voltage is controlled by the voltage control circuit 15 so as to maintain the required voltage.

FIG. 2 schematically shows an example of a hydride gas quantification device for detecting and quantifying sulfur and phosphorus hydride gases. The hydride gas conveyed to the hydride gas quantification device 12 is introduced into the gas contact chamber 19 through the gas introduction pipe 18, and the suction pump 2 from the gas discharge pipe 20.
Exhausted through 1. At the bottom of the gas contact chamber 19, H
_{A 2} S detecting test paper 22 and a PH ₃ detecting test paper 23 are provided, and an irradiation lamp 24 and a photodiode 25 are attached to the upper parts of both test papers. The photodiode 25 is a color intensity detection device 2 including a microcomputer.
Connected to 6. H ₂ S detection test paper 22 and P
The test strip 23 for H ₃ detection corresponds to each test strip running device 2
The traveling speed is adjusted by 7 and the tape travels between the rewind reel 28 and the take-up reel 29 on which the tape-shaped test paper is wound.

The hydride gas conveyed to the gas contact chamber 19 comes into contact with the H ₂ S detecting test paper 22 and the PH ₃ detecting test paper 23, and the gas contact surface of the H ₂ S detecting test paper 22 The lead acetate impregnated in the test paper reacts with H ₂ S to produce lead sulfide (black), and the PH ₃ detection test paper 23
On the gas contact surface of the test paper, silver nitrate and PH impregnated in the test paper
₃ reacts and silver precipitation (brown) occurs respectively. It is possible to know the H ₂ S and PH ₃ concentrations detected on the test paper by irradiating the colored portion of each test paper with monochromatic light from the irradiation lamp 24 and detecting the reflected light intensity with the photodiode 25. When H ₂ S and PH ₃ coexist, H ₂
S detection test paper detects only H ₂ S, PH ₃ does not detect any, PH ₃ detection test paper would also detects H ₂ S detects the PH _3. H of the test paper for detecting PH _{3
Since the} detection sensitivity to ₂ S is 1/10 or less of PH ₃ , if the H ₂ S concentration is 1/10 or less of the PH ₃ concentration, the method of contacting the hydride gas with the test paper shown in this example is used for sulfur and phosphorus. Can be quantified sufficiently.

However, when the H ₂ S concentration is high, the contact method shown in this example may cause a large error in the quantitative value. In this case, it is preferable that the hydride gas is brought into contact with the H ₂ S detection test paper and then brought into contact with the PH ₃ detection test paper. By contacting the hydride gas with the H ₂ S detection test paper to consume the entire amount of H ₂ S, and then contacting the PH ₃ detection test paper, both hydride gases can be removed without interfering components. It becomes possible to detect.

FIG. 3 schematically shows an example of a hydride gas quantification device for carrying out this. The hydride gas introduced into the gas contact chamber 19 through the gas introduction pipe 18 first passes from one side of the H ₂ S detection test paper 22 to the opposite side, and then from one side of the PH ₃ detection test paper 23. The gas passes through in the opposite direction and is discharged through the gas discharge pipe 20 and the suction pump 21. An irradiation lamp 24 and a photodiode 25 are attached to the upper part of the gas inflow surface of each test paper, and the photodiode 25 is connected to a color development intensity detection device 26 including a microcomputer. The hydride gas introduced into the gas contact chamber 19 is used in the rewind reel 2
By passing both test papers that run between the roll 8 and the take-up reel 29, color is developed on the inflow surface. The H ₂ S and PH ₃ concentrations can be known by irradiating the colored portion with monochromatic light from the irradiation lamp 24 and detecting the intensity of the reflected light with the photodiode 25.

Using this hydride gas quantitative analyzer, H
_{Even when 2} S and PH ₃ coexist, both hydride gases can be detected and quantified in the absence of interfering components. In this example, when the H ₂ S is present in very high concentrations, H ₂ S the total amount can not be consumed by H ₂ S detection test paper, PH in PH ₃ detection test strip
₃ May affect detection. In such a case, the gas that has passed through the H ₂ S detection test strip is passed through the lead acetate filter 30 to completely remove only H ₂ S, and then contact or pass through the PH ₃ detection test strip. You can do it.

Further, in order to make the contact structure between the hydride gas and the test paper simpler, it is possible to detect the hydride gas by superposing both test papers. FIG. 4 shows an example of the hydride gas quantification device. H ₂ S detection test paper and P
The H ₃ detection test papers are superposed and supplied to the lower part of the gas contact chamber 19, and the hydride gas introduced into the gas contact chamber 19 through the gas introduction pipe 18 is PH ₃ from the upper surface of the H ₂ S detection test paper. Gas exhaust pipe 2 that passes through the bottom surface of the test strip for detection
0, discharged through the suction pump 21. The H ₂ S detecting test paper and the PH ₃ detecting test paper are respectively used by the test paper running device 27 to rewind the reel 28 and the take-up reel 2.
The test strips are separated after contact with hydride gas, and monochromatic light is radiated from the irradiation lamp 24 to the color-developed portions on the respective gas inflow surfaces. Detected by the photodiode 25, the H ₂ S and PH ₃ concentrations are measured. Also in this example, since the hydride gas is detected by the H ₂ S detecting test strip and then by the PH ₃ detecting test strip, even if H ₂ S and PH ₃ coexist, they are affected by each other. It is possible to detect and quantify each without.

Here, a method for simultaneously quantifying sulfur and phosphorus using the hydride gas generator configured as shown in FIG. 1 and the hydride gas quantification device configured as shown in FIG. 3 will be described. To do. Sample 10 is a cylindrical steel having a diameter of 30 mm and a height of 20 mm. The sample 10 is placed on the top of the reaction chamber 2, and the sample electrode 14 is brought into contact therewith. 6M HCl which is an electrolyte by driving the electrolyte pump 8
Are continuously supplied to the reaction chamber 2. On the way, HC1 is heated to 100 ° C. by the heat exchanger 9. In this state,
While applying an electrolytic voltage (0.7 V) to the sample 10,
Nitrogen gas is supplied from the nitrogen gas cylinder 3 to the reaction chamber 2 at a constant flow rate (100 ml / min). Sulfur and phosphorus in the sample 10 are reduced to H ₂ S and PH ₃ , respectively, and enter the gas-liquid separator 6 along with the nitrogen gas. In the gas-liquid separator 6, HC
1 returns to the electrolyte tank 7, and H ₂ S and PH ₃ are sent to the hydride quantification device 12 together with nitrogen gas. On the way
The line filter 11 removes HCl mist.

In the hydride gas meter 12, the H ₂ S detecting test paper 22 and the PH ₃ detecting test paper 23 are continuously fed at a constant speed (4 cm / min). The H ₂ S and PH ₃ sent together with the nitrogen gas first pass through the H ₂ S detection test paper 22. The test paper 22 for H ₂ S detection does not detect PH ₃ at all and selectively detects only H ₂ S,
Color development according to the H ₂ S concentration is exhibited on the test paper. The gas that has passed through the H ₂ S detecting test paper 22 flows into the lead acetate filter 30 after passing through the test paper. The lead acetate filter 30 is not necessary when there is no possibility that 100 ppm or more of H ₂ S will be conveyed. However, in this example, since a high concentration of H ₂ S may have been conveyed, acetic acid is used. A lead filter 30 was installed. H ₂ S H ₂ S remaining in the gas passing through the detection test paper 22 is lead acetate filter 30
Lead sulphide is produced in it and is adsorbed on the filter. On the other hand, since PH ₃ in the carrier gas does not react with lead acetate, it is not adsorbed on the lead acetate filter 30, and as a result, PH ₃ detection test paper 2
Only PH ₃ is sent to _3, and the color is developed according to the PH ₃ concentration. The colored portions on the H ₂ S detecting test paper 22 and the PH ₃ detecting test paper 23 are illuminated by the irradiation lamp 24, and after the reflected light intensity is detected by the photodiode 25, the color developing intensity is detected by the color developing intensity detecting device 26. Ie H
₂ S and PH ₃ concentrations are calculated.

FIG. 5 shows the measurement of the reflected light intensity of the H ₂ S detecting test strip and the PH ₃ detecting test strip when H ₂ S and PH ₃ were generated by electrolysis using the above block steel sample. The results are shown. When the electrolysis is started, the intensity of the reflected light on both test papers immediately decreases and stabilizes in about 1 minute. After that, during the electrolysis, both test papers show almost constant reflected light intensity, and when the electrolysis is stopped, the reflected light intensity immediately changes and returns to the initial reflected light intensity. By previously determining the relationship between the reflected light intensity during electrolysis and the sulfur and phosphorus content, sulfur and phosphorus can be quantified at the same time.

[0026]

EFFECTS OF THE INVENTION According to the present invention, it is possible to simultaneously and rapidly perform the quantification of sulfur and phosphorus in a metal sample which has required complicated analysis operations and required a long analysis time. Moreover, since the test paper photoelectric photometric method capable of detecting the hydride gas of sulfur and phosphorus with high sensitivity is used as the gas analyzer, sulfur and phosphorus up to ppm order can be quantified. Therefore, it has a great effect on the fields such as metal refining, operation control in the metal manufacturing industry such as steel manufacturing process, or product quality control.

[Brief description of drawings]

FIG. 1 is an apparatus configuration diagram showing an example of a hydride gas generator in a quantitative analysis apparatus for carrying out the method of the present invention.

FIG. 2 is a device configuration diagram showing an example of a hydride gas quantification device in a quantification analysis device for carrying out the method of the present invention.

FIG. 3 is an apparatus configuration diagram showing another example of a hydride gas quantification apparatus in the quantitative analysis apparatus for carrying out the method of the present invention.

FIG. 4 is an apparatus configuration diagram showing still another example of the hydride gas quantification device in the quantitative analysis device for carrying out the method of the present invention.

FIG. 5 is a diagram showing an example of the results of measurement of reflected light intensities of the H ₂ S detection test paper and the PH ₃ detection test paper.

[Explanation of symbols]

1 Hydride gas generator 2 Reaction chamber 3 Nitrogen gas cylinder 4 Needle valve 5 Flow meter 6 Gas-liquid separator 7 Electrolyte tank 8 Electrolyte pump 9 Heat exchanger 10 Sample 11 Line filter 12 Hydride gas quantifier 13 Electrolyzer 14 Sample electrode 15 Voltage control circuit 16 Power supply 17 Voltage measurement circuit 18 Gas introduction pipe 19 Gas contact chamber 20 Gas discharge pipe 21 Suction pump 22 H ₂ S detection test paper 23 PH ₃ detection test paper 24 Irradiation lamp 25 Photodiode 26 Color intensity detector 27 Test paper running device 28 Rewinding reel 29 Take-up reel 30 Lead acetate filter

Claims (5)

[Claims] 1. A hydrogen gas in which a hydride gas exists while a metal sample is reacted with an acid having an electrolysis or reducing power in a hydride gas generator to generate a hydride gas of sulfur and phosphorus in the sample. In a method for quantifying sulfur and phosphorus in a metal sample by supplying an inert gas into a hydride gas generator and guiding the hydride gas together with the inert gas to a hydride gas quantification device, the PH ₃ detection test paper impregnated with a reagent that exhibits coloration produced H ₂ S and the chemical reaction H ₂ S detection test paper and PH ₃ and chemical reaction of the reagent impregnated exhibiting the resulting color development in gas contact chamber The sulfur and phosphorus in a metal sample are characterized in that the hydride gas is supplied to each of the test papers to bring the test papers into color, and the color development intensity is measured to simultaneously determine sulfur and phosphorus. Simultaneous analysis method of phosphorus. 2. The method according to claim 1, wherein the hydride gas comes into contact with the test paper for detecting H ₂ S and then with the test paper for detecting PH _{3 in} the gas contact chamber of the hydride gas quantification device. Method for simultaneous analysis of sulfur and phosphorus in metal samples. 3. A hydride gas generator for generating H ₂ S and PH ₃ from a metal sample, a device for supplying an inert gas into the hydride gas generator in which the hydride gas is present, and an inert gas An analyzer equipped with a hydride gas quantification device for quantifying the introduced hydride gas, wherein the hydride gas quantification device is impregnated with a reagent that causes a chemical reaction with H ₂ S to develop color and detects H ₂ S. It includes a use test strips and PH ₃ and PH ₃ detection test paper impregnated with a reagent that exhibits coloration caused a chemical reaction, comprising a further two test paper with the gas contact chamber hydride gas contacts, and each test paper Sulfur in a metal sample characterized by being equipped with a color intensity detector capable of measuring the concentrations of sulfur and phosphorus by irradiating monochromatic light on the gas contact surface of Simultaneous phosphorus analyzer. 4. A hydride gas quantification device supplies an H ₂ S detecting test strip into the gas transport path to pass the entire amount of the transport gas from one side of the test strip to the opposite side, and It is equipped with a gas contact chamber with a structure that allows the entire amount to pass from one side of the PH ₃ detection test paper to the opposite side, and irradiates monochromatic light on the gas inflow surface of each test paper and detects the reflected light intensity to detect sulfur. 4. The simultaneous analysis device for sulfur and phosphorus in a metal sample according to claim 3, further comprising a color development intensity detection device capable of measuring the concentration of phosphorus. 5. A hydride gas quantification device supplies a test strip for PH ₃ detection under a test strip for H ₂ S detection in a gas transport path, and supplies the total amount of the transport gas for H ₂ S detection. It is equipped with a gas contact chamber with a structure that passes from the top surface of the test paper to the bottom surface of the PH ₃ detection test paper, and after separating each test paper, irradiates the gas inflow surface of each test paper with monochromatic light and reflects it. 4. The simultaneous analyzer for sulfur and phosphorus in a metal sample according to claim 3, further comprising a color development intensity detector capable of detecting the intensity and measuring the concentrations of sulfur and phosphorus.