JP2008164513A - Measuring period determining method, icp emission spectrometer analyzer and program - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a measuring period determinating method more accurately determinating the measuring period of a sample, an ICP emission spectrometer, and a program that makes the ICP emission spectrometer to function. <P>SOLUTION: The input part 83 of the ICP emission analyzer 1 receives the input a monitor element and a central control part 8 acquires the emission intensity related to the received element via a detector 12. The measuring period of the sample is determined on the basis of the acquired emission intensity. The washing completion period of a sample is determined, on the basis of the emission intensities acquired after the measuring period of the sample is determined. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a measurement timing discriminating method for discriminating the measurement timing of a sample by an ICP emission analyzer that measures the emission intensity of an element in the sample, an ICP emission analyzer, and a program for causing the ICP emission analyzer to function.

  An elemental analyzer using a high frequency inductively coupled plasma (ICP) as a light source is known. High frequency inductively coupled plasma is plasma generated by high frequency induction. An ICP light source generally forms a plasma by winding an induction coil around a quartz tube called a plasma torch to flow a high-frequency current (for example, 27.12 MHz) to generate an induction electric field and introducing argon gas into the plasma torch. To do. A mist-like sample is fed into the plasma by an argon carrier gas.

  Since the temperature of the plasma is usually several thousand degrees to 10,000 degrees, light emission occurs at a wavelength specific to the element in the sample. In these emission spectra, light having a target wavelength is selected by a spectroscope including a diffraction grating or a prism, and the emission intensity is measured by, for example, a photomultiplier tube. Usually, emission intensity is measured for several seconds to several minutes for one wavelength, and the obtained value is converted into a concentration or the like by a data processing unit (see, for example, Patent Document 1).

  By the way, stabilization time is an important item for analyzing a sample. The stabilization time includes, for example, the stabilization time of the power source, the stabilization time of plasma, and the stabilization time at the time of sample exchange. Samples are analyzed after this stabilization time. Among the stabilization times, the stabilization time of the power source and the stabilization time of the plasma can be determined quantitatively according to the conditions and installation environment specific to the apparatus.

  Conventionally, regarding the stable time at the time of sample exchange, the time that the air mixed in when transferring the introduction tube to the container containing the sample reaches the plasma torch and the fog density of the atomized sample are constant. It was only empirically grasping the time to become. That is, conventionally, after the sample was introduced, the time until the sample reached the plasma torch was empirically grasped, and the analysis was only started as the stable time at the time of sample replacement.

When the measurement of the sample is completed and the next sample is measured, the inside of the apparatus is cleaned with distilled water. In order to prevent contamination in the apparatus and improve the measurement accuracy, the apparatus needs to be thoroughly cleaned. Conventionally, it has been empirically determined that the cleaning has been completed, and then the next sample has been introduced.
Japanese Patent Laid-Open No. 8-145892

  However, the conventional method has only empirically determined the stabilization time at the time of exchanging samples, and has not been accurate. That is, there is a problem that there is no clear standard at the start of measurement. In particular, when a small amount of sample is introduced, there is a problem that the sample cannot be sufficiently analyzed due to a delay in measurement start timing.

  In addition, since the cleaning end time has been determined empirically in the past, the next sample may be introduced even though the cleaning has not been completed completely. The measurement error due to the accumulation of was invited. In particular, when mercury or boron having a large memory action is present in the sample, the influence is great.

  The present invention has been made in view of such circumstances, and its purpose is to receive an input of an element to be monitored, and to determine the measurement timing of a sample based on the emission intensity related to the received element, thereby making it more accurate. An object of the present invention is to provide a measurement timing discriminating method capable of discriminating the measurement timing of a sample, an ICP emission analyzer, and a program for causing the ICP emission analyzer to function.

  Another object of the present invention is to determine the cleaning end time of the sample based on the obtained emission intensity after determining the measurement time of the sample, so that it is possible to easily determine the cleaning end time of the sample, and then quickly. An object of the present invention is to provide a measurement time determination method capable of measuring the next sample.

  Another object of the present invention is to identify the element in the sample by analyzing the composition of the sample based on the emission intensity corresponding to each element output from the spectrometer before receiving the input of the element to be monitored. Another object of the present invention is to provide a measurement time discriminating method capable of discriminating the measurement time of an element by receiving one or more elements in a sample as an element to be monitored.

  The measuring time discriminating method according to the present invention is a measuring time discriminating method for discriminating the measuring time of a sample by an ICP emission spectrometer that measures the luminescence intensity of the element in the sample. An acquisition step of acquiring luminescence intensity related to the element received in the reception step, and a determination step of determining the measurement timing of the sample based on the luminescence intensity acquired in the acquisition step are provided.

  The measurement timing determination method according to the present invention further includes an end timing determination step of determining the cleaning end timing of the sample based on the emission intensity acquired by the acquisition step after determining the measurement timing of the sample by the determination step. It is characterized by that.

  In the measurement timing determination method according to the present invention, the determination step includes a change determination step for determining whether or not a temporal change in the emission intensity acquired in the acquisition step is greater than a predetermined value, and the predetermined determination by the change determination step. A range determination step for determining whether or not a temporal change in the emission intensity acquired in the acquisition step is within a predetermined range when it is determined that the value is greater than a value; and a determination as to be within the predetermined range by the range determination step And a step of discriminating that it is time to measure the sample.

  In the measurement time determination method according to the present invention, the end time determination step determines whether or not the temporal change in the emission intensity acquired by the acquisition step is greater than a predetermined value after the measurement time of the sample is determined by the determination step. A step of determining whether or not a temporal change in the light emission intensity acquired by the acquisition step is within a predetermined range when the step determines that the value is larger than the predetermined value. A step of discriminating that it is the cleaning end timing of the sample when it is discriminated that it is within the predetermined range.

  The measurement time determination method according to the present invention further includes an analysis step of analyzing the composition of the sample based on the emission intensity corresponding to each element output from the spectrometer before receiving the input of the element to be monitored in the receiving step. The receiving step is characterized in that the element in the sample analyzed by the analyzing step is received as an element to be monitored.

  The measurement time determination method according to the present invention further includes a step of adding an element other than the measurement target when the contained element of the sample is unknown, and the receiving step receives the added element as an element to be monitored. Features.

  An ICP emission analysis apparatus according to the present invention is an ICP emission analysis apparatus that measures the emission intensity of an element in a sample, and receives an input of an element to be monitored and obtains the emission intensity of the element received by the reception means. And obtaining means for judging the measurement timing of the sample based on the emission intensity obtained by the obtaining means.

  The ICP emission analysis apparatus according to the present invention further includes an end timing determination unit that determines the cleaning end timing of the sample based on the emission intensity acquired by the acquisition unit after the determination unit determines the measurement time of the sample. It is characterized by that.

  In the ICP emission analysis apparatus according to the present invention, the determination means includes a change determination means for determining whether or not a temporal change in the emission intensity acquired by the acquisition means is greater than a predetermined value, and the predetermined change by the change determination means. When it is determined that the value is larger than the value, a range determination unit that determines whether or not the temporal change in the emission intensity acquired by the acquisition unit is within a predetermined range; and the range determination unit determines that the change is within the predetermined range And a means for discriminating that it is the measurement time of the sample.

  In the ICP emission analysis apparatus according to the present invention, the end time determination unit determines whether or not the temporal change in the emission intensity acquired by the acquisition unit is greater than a predetermined value after the determination unit determines the measurement time of the sample. Means for determining whether or not the temporal change in the emission intensity acquired by the acquisition means is within a predetermined range when the means determines that the value is greater than the predetermined value, and the means And a means for determining that it is the cleaning end time of the sample when it is determined to be within the predetermined range.

  The ICP emission analysis apparatus according to the present invention further comprises an analyzing means for analyzing the composition of the sample based on the emission intensity corresponding to each element output from the spectrometer before receiving the input of the element to be monitored by the receiving means. The receiving means is configured to receive an element in the sample analyzed by the analyzing means as an element to be monitored.

  The program according to the present invention is a program for discriminating the measurement time of a sample by an ICP emission analyzer that measures the emission intensity of an element in the sample, and accepting an input of the element to be monitored to the ICP emission analyzer; The acquisition step of acquiring the emission intensity related to the element received in the reception step and the determination step of determining the measurement time of the sample based on the emission intensity acquired in the acquisition step are performed.

  The program according to the present invention further executes an end timing determination step of determining a cleaning end timing of the sample based on the emission intensity acquired by the acquisition step after determining the measurement timing of the sample by the determination step. Features.

  In the present invention, the receiving means receives an input of the element to be monitored. The light emission intensity related to the accepted element is obtained by the obtaining means. The discriminating unit discriminates the measurement time of the sample based on the emission intensity acquired by the acquiring unit. This determination is made, for example, by determining whether or not the temporal change in the emission intensity acquired by the acquisition unit is greater than a predetermined value, and when it is determined that the temporal change is greater than the predetermined value, the temporal change in the emission intensity acquired by the acquisition unit Is determined to be within a predetermined range. When it is determined that the temporal change in the emission intensity is within the predetermined range, it is determined that it is the measurement time of the sample.

  Further, for example, when the emission intensity acquired by the acquisition unit exceeds a threshold stored in advance, the determination is made as the measurement time of the sample. Since it comprised in this way, it becomes possible to discriminate | determine the measurement time of a sample accurately.

  In the present invention, the end time determination means determines the cleaning end time of the sample based on the emission intensity acquired by the acquisition means after the determination time of the sample is determined by the determination means. This determination is performed by, for example, determining whether the temporal change in the emission intensity acquired by the acquisition unit is greater than a predetermined value after determining the measurement time of the sample by the determination unit. It is determined whether or not the temporal change in the emission intensity acquired by the acquisition means is within a predetermined range. When it is determined that the temporal change in the emission intensity is within the predetermined range, it is determined that it is the cleaning end time of the sample.

  In the present invention, qualitative analysis is performed in advance based on the emission intensity corresponding to each element output from the spectrometer. Since the composition of the sample is analyzed by this, it is possible to measure the elements in the sample by this analysis, and then select the optimum element as the element to be monitored, and determine the measurement time of the sample at the optimum timing. . The element to be monitored is an element that, when at least one of the elements in the sample is known, is selected from at least one of the known elements and whose emission intensity change is monitored to determine the measurement timing. When the element in the sample is not known at all, if the element to be measured is determined, an arbitrary element other than the element to be measured can be added to the sample, and the added sample can be selected as an element to be monitored. In addition, if you want to analyze the elements of the sample, you can select the element to be monitored from the results of the qualitative analysis analyzed in advance when performing the quantitative analysis after the qualitative analysis that analyzes the composition contained in the sample. it can.

  In the present invention, the receiving unit receives an input of an element to be measured, and acquires the emission intensity related to the received element by the acquiring unit. Since the determination means determines the measurement timing of the sample based on the temporal change in the emission intensity acquired by the acquisition means, for example, when the temporal change in the emission intensity of the element to be monitored is larger than a predetermined value, the predetermined range It is possible to determine the measurement timing of the sample with high accuracy, for example, by determining that the sample is stable when it falls within, and starting elemental analysis (so-called qualitative analysis or quantitative analysis) of the measurement target. Thereby, it becomes possible to start the measurement of the sample at the optimum timing regardless of the user's experience. If it is unclear whether the element to be monitored is contained in the sample, the same effect can be obtained by adding any element other than the sample to be measured to the sample and using the element as the monitor element to observe the change in emission intensity. can get.

  In the present invention, the end time determination means determines the sample cleaning end time based on the temporal change in the emission intensity acquired by the acquisition means after the measurement time of the sample is determined by the determination means. It becomes possible to more accurately recognize the cleaning end time of the sample that has been measured. Accordingly, it is possible to recognize the cleaning end time more accurately regardless of whether or not the user has experience, and to prevent contamination in the apparatus and occurrence of measurement errors. In particular, the effect is greater when measuring a sample having a larger memory effect that takes longer to clean the sample than other elements such as mercury or boron.

  In the present invention, if a qualitative analysis is performed based on the emission intensity corresponding to each element output from the spectrometer before receiving the element to be monitored, the element in the sample by this analysis can be measured. The present invention has an excellent effect, for example, that it is possible to determine the measurement timing of the sample at an optimal timing when performing analysis.

Embodiment 1
FIG. 1 is a block diagram showing a hardware configuration of an ICP emission analyzer according to the present invention. The ICP emission analyzer 1 includes a plasma torch 2, a high frequency power source 3, a high frequency coil 5, a gas control unit 6, a sample introduction unit 7, a pump 9, an introduction tube 10, a spectrometer 11, a detector 12, a spectrometer control unit 112, And it is comprised including the central control part 8 as an acquisition means.

  Argon gas flows through the plasma torch 2, and a high frequency is supplied from a high frequency power source 3 to a high frequency coil 5 surrounding the plasma torch 2, thereby generating plasma 4. As the sample to be analyzed, for example, a solution containing Fe or a solution containing Ni is used. Distilled water for washing is stored in a distilled water container 13 and is sucked by a pump 9 through an introduction pipe 10 and guided to a sample introduction unit 7.

  The sample is stored in the sample container 14, and when the analysis of the sample is started, the introduction tube 10 inserted in the distilled water container 13 is transferred to the sample container 14. When the introduction tube 10 is inserted into the sample container 14, the sample is sucked by the pump 9 through the introduction tube 10 and guided to the sample introduction unit 7. In the present embodiment, a description will be given of a mode in which the introduction tube 10 is manually transferred between the distilled water container 13 and the sample container 14, but it may be automatically transferred using, for example, an autosampler.

  Distilled water, air and sample introduced into the sample introduction unit 7 are atomized and sent to the plasma torch 2. The gas flow rate of the gas flowing in the plasma torch 2 and the gas used for atomizing the sample in the sample introduction unit 7 is controlled by the gas control unit 6. Measurement conditions such as high-frequency output and gas flow rate are controlled by the central control unit 8.

  Light emission generated by the plasma 4 reaches the detector 12 through the spectroscope 11. The detector 12 converts the light having a specific wavelength dispersed by the spectroscope 11 into an electric signal, and amplifies the electric signal by an amplifier circuit (not shown). The amplified electric signal is digitized and output to the central control unit 8 as information about the light intensity (light emission intensity). The spectroscope 11 includes a diffraction grating 111 or a prism inside and extracts light of a specific wavelength. The spectroscope control unit 112 is connected to the central control unit 8 and the spectroscope 11, and controls the rotation of the diffraction grating 111 in the spectroscope 11 according to an instruction from the central control unit 8. In the present embodiment, a mode using a monochromator as the spectroscope 11 will be described, but a polychromator may be used.

  The central control unit 8 is, for example, a personal computer, and includes a CPU (Central Processing Unit) 81, a RAM (Random Access Memory) 82, a storage unit 85, an input unit 83, and a display unit 84, and outputs from the detector 12. Based on the information, various data processing, control of the spectroscope control unit 112, and control of various hardware such as the sample introduction unit 7 are performed. In this embodiment, various processes are performed by a personal computer. However, these processes may be realized by hardware such as an integrated circuit.

  The CPU 81 is connected to each hardware unit of the central control unit 8 via the bus 87, and controls them, and executes various software functions according to a control program stored in the storage unit 85 such as a hard disk. . The control program is described in a programming language such as C language.

  The RAM 82 is configured by SRAM (Static Random Access Memory), flash memory, or the like, and stores temporary data generated during execution of software. The input unit 83 includes, for example, a keyboard and a mouse, and outputs information input by the user to the CPU 81. The display unit 84 is configured by an LCD (Liquid Crystal Digital) display or the like, and displays various information such as the analysis start time based on instructions from the CPU 81. Note that the input unit 83 and the display unit 84 may be configured integrally with a touch panel.

  In order to clean the inside of the plasma torch 2, the sample introduction part 7, the introduction tube 10, etc., distilled water is introduced from the introduction tube 10 prior to the measurement of the sample. Here, the user inputs an element to be monitored (hereinafter referred to as a monitor element) from the input unit 83. When at least one element contained in the sample is known, at least one monitor element may be selected from the known elements and used as the monitor element. In this case, when a known contained element includes an element to be measured, if the element is a monitor element, it is possible to save the trouble of measuring twice. When the contained element in the sample is unknown, an arbitrary element other than the element to be measured may be added to the sample, and the added sample may be used as the monitor element. The CPU 81 accepts input of an element to be measured input from the input unit 83. The CPU 81 outputs the received element information to the spectrometer control unit 112. The spectroscope control unit 112 rotates the diffraction grating 111 to an angle corresponding to the received element. Subsequently, the user transfers the introduction tube 10 from the distilled water container 13 to the sample container 14. FIG. 2 is a graph showing temporal changes in the emission intensity output from the detector 12. In FIG. 2, the horizontal axis indicates time, and the vertical axis relatively indicates the light emission intensity.

  In this embodiment, it is assumed that an input of iron (Fe) is accepted as a monitor element. Note that the CPU 81 may read the periodic table of chemical symbols from the storage unit 85 and display the chemical symbol on the display unit 84, and may accept an element selected by the user from the input unit 83 as a monitor element. The graph of FIG. 2 shows the temporal change in the emission intensity of iron output from the detector 12 when the diffraction grating 111 is rotated to an angle for detecting the wavelength of iron. It can be understood that a sample containing iron was introduced next to distilled water, the emission intensity increased rapidly after about 10 seconds, and the emission intensity became stable after about 15 seconds.

  The central control unit 8 performs the following processing to determine the introduction time. The CPU 81 of the central control unit 8 calculates a temporal change in the output light emission intensity, and determines whether or not it is larger than a predetermined value stored in the storage unit 85 in advance. After the sample containing iron is introduced, the emission intensity changes rapidly with time. When the temporal change is larger than a predetermined value, the CPU 81 determines whether or not the temporal change in the light emission intensity is within a predetermined range for a predetermined time. For example, the CPU 81 calculates a standard deviation value or dispersion value of the light emission intensity within a predetermined time, and determines whether or not this is equal to or less than a standard deviation value or dispersion value serving as a reference stored in the storage unit 85. Hereinafter, an example using standard deviation values will be described.

  When the CPU 81 determines that the temporal change in the light emission intensity is within the predetermined range for a predetermined time, it determines that the measurement is stable, that is, the measurement time has been reached, reads a predetermined message from the storage unit 85, and displays it on the display unit 84. To do. This message may be, for example, “Measurement can be started”. Thereafter, measurement of elements contained in the sample (qualitative analysis) or analysis of how much of the element to be measured that has been determined in advance (quantitative analysis) is started.

  After the predetermined measurement, the user transfers the introduction tube 10 from the sample container 14 to the distilled water container 13. As shown in FIG. 2, it can be understood that the cleaning of the sample containing iron proceeds after about 40 seconds, and the cleaning is completed after about 60 seconds. After the CPU 81 determines that the temporal change in the light emission intensity is within a predetermined range for a predetermined time, the CPU 81 calculates the temporal change in the output light emission intensity and is larger than a predetermined value stored in the storage unit 85 in advance. Determine whether or not.

  After distilled water is introduced instead of the sample containing iron, the emission intensity decreases rapidly with time. When the temporal change is larger than a predetermined value, the CPU 81 determines whether or not the temporal change in the light emission intensity is within a predetermined range for a predetermined time. For example, the CPU 81 calculates a standard deviation value of the light emission intensity within a predetermined time and determines whether or not the standard deviation value stored in the storage unit 85 is equal to or less than the standard deviation value as in the process described above. When the CPU 81 determines that the temporal change in the emission intensity is within the predetermined range for a predetermined time, it determines that the cleaning end time has been reached, reads a predetermined message from the storage unit 85, and displays it on the display unit 84. This message may be, for example, “Next sample can be introduced” or “Washing is completed”.

  The determination process of the measurement time and the cleaning end time in the above hardware configuration will be described using a flowchart. FIG. 3 is a flowchart showing the determination process of the measurement time and the cleaning end time. Prior to the introduction of the sample, the user inputs a monitor element from the input unit 83. CPU81 receives the input of the monitor element inputted from input part 83 (Step S31). The CPU 81 outputs the received element information to the spectrometer control unit 112. The spectroscope control unit 112 rotates the diffraction grating 111 to an angle corresponding to the received element (step S32).

  The central control unit 8 acquires the emission intensity output from the detector 12 (step S33). The CPU 81 sequentially stores the acquired light emission intensity in the RAM 82, calculates a temporal change in the light emission intensity, and determines whether or not the light emission intensity is greater than a predetermined value stored in advance in the storage unit 85 (step S34). If the CPU 81 determines that the temporal change in the emission intensity is smaller than the predetermined value (NO in step S34), it determines that distilled water is still being supplied, and repeats the process in step S34.

  On the other hand, when the CPU 81 determines that the temporal change in the emission intensity is greater than the predetermined value (YES in step S34), the CPU 81 determines that the sample has started to be supplied, and the temporal change in the emission intensity within the predetermined time is the storage unit 85. It is determined whether it is within the range of the standard deviation value stored in advance (step S35). If the CPU 81 determines that the temporal change in the light emission intensity is not within the standard deviation value range (NO in step S35), the CPU 81 repeats the process in step S35, assuming that the stable time has not been reached. On the other hand, if the CPU 81 determines that the temporal change in the emission intensity is within the standard deviation value range (YES in step S35), the CPU 81 determines that it is the measurement time and displays the message read from the storage unit 85 on the display unit 84. (Step S36).

  Thereafter, the CPU 81 determines whether or not the temporal change in the light emission intensity is larger than a predetermined value stored in advance in the storage unit 85 (step S37). If the CPU 81 determines that the temporal change in the emission intensity is smaller than the predetermined value (NO in step S37), the CPU 81 determines that the sample supply is continued, and repeats the process in step S37.

  On the other hand, when the CPU 81 determines that the temporal change in the emission intensity is greater than the predetermined value (YES in step S37), the CPU 81 determines that distilled water has started to be supplied instead of the sample, and the temporal change in the emission intensity within the predetermined time. Is within the range of the standard deviation value stored in advance in the storage unit 85 (step S38). The standard deviation value may be a value smaller than the standard deviation value read from the storage unit 85 in step S35. When the CPU 81 determines that the temporal change in the light emission intensity is not within the standard deviation value range (NO in step S38), the CPU 81 repeats the process in step S38, assuming that the cleaning has not been completed yet. On the other hand, if the CPU 81 determines that the temporal change in the light emission intensity is within the standard deviation value range (YES in step S38), it determines that it is the cleaning end time, and displays the message read from the storage unit 85 on the display unit 84. (Step S39).

Embodiment 2
In the first embodiment, it is determined whether or not the temporal change in the emission intensity is greater than a predetermined value, and then it is determined whether or not the temporal change in the emission intensity is within a predetermined range. If the emission intensity of at least one of the elements contained in the sample is known, such as by performing a quantitative analysis after the measurement, a rough emission intensity obtained by qualitative analysis or the like is set as a threshold value and stored in advance as in the second embodiment. The determination may be made based on the threshold value.

  FIG. 4 is a flowchart showing the determination process of the measurement time and the cleaning end time according to the second embodiment. Prior to the introduction of the sample, the user inputs a monitor element from the input unit 83. CPU81 receives the input of the monitor element input from input part 83 (Step S41). The CPU 81 outputs the received element information to the spectrometer control unit 112. The spectroscope controller 112 rotates the diffraction grating 111 to an angle corresponding to the received element (step S42).

  The central controller 8 acquires the light emission intensity output from the detector 12 (step S43). CPU81 reads a threshold value from the memory | storage part 85 (step S44). In this case, an appropriate emission intensity is input from the input unit 83 as a threshold value. The CPU 81 determines whether or not the light emission intensity is greater than or equal to the read threshold value (step S45). When the CPU 81 determines that the light emission intensity is not equal to or greater than the threshold (NO in step S45), the CPU 81 repeats the process of step S45 assuming that the stable time has not been reached. On the other hand, when the CPU 81 determines that the light emission intensity is equal to or higher than the threshold (YES in step S45), the CPU 81 determines that it is the measurement time and displays the message read from the storage unit 85 on the display unit 84 (step S46).

  Thereafter, the CPU 81 reads the threshold value from the storage unit 85 (step S47). This threshold value may be different from the threshold value read in step S44. The CPU 81 determines whether or not the emission intensity is equal to or less than the read threshold value (step S48). If the CPU 81 determines that the emission intensity is not less than or equal to the threshold value (NO in step S48), the process of step S48 is repeated assuming that the cleaning has not ended. On the other hand, when the CPU 81 determines that the light emission intensity is equal to or lower than the threshold value (YES in step S48), it determines that it is the cleaning end time, and displays the message read from the storage unit 85 on the display unit 84 (step S49). Note that the processing of the first embodiment and the processing of the second embodiment may be combined. For example, the determination based on the standard deviation value is performed, for example, the determination of the measurement time is performed using the processing of step S34 and step S35 according to the first embodiment, and the determination of the cleaning end time is performed using the processing of step S48 according to the second embodiment. And discrimination using a threshold value may be appropriately combined.

  The second embodiment is configured as described above, and the other configurations and operations are the same as those of the first embodiment. Therefore, corresponding parts are denoted by the same reference numerals, and detailed description thereof is omitted.

Embodiment 3
Qualitative analysis, that is, analysis of the composition of elements in the sample in advance, may be performed after the measurement timing and cleaning end timing described in the first or second embodiment. FIG. 5 is a block diagram showing a hardware configuration of the ICP emission spectrometer 1 according to the third embodiment. In addition to the configuration of the first embodiment, the storage unit 85 stores a qualitative analysis file 851 obtained by qualitative analysis. FIG. 6 is an explanatory diagram showing a record layout of the qualitative analysis file 851. For example, the qualitative analysis file 851 includes an element field, a comparative emission intensity field, and a rotation angle field associated with the wavelength. In the element field, a plurality of elements obtained by qualitative analysis are stored. In the comparative light emission intensity field, a comparative light emission intensity serving as a threshold is stored in association with the element. In the rotation angle field, the rotation angle of the diffraction grating 111 when detecting the emission intensity of the element is stored in correspondence with the element. The unit is degrees.

  When the CPU 81 determines that the emission intensity is greater than the comparative emission intensity, the CPU 81 determines that the corresponding element is included in the sample. In the example of FIG. 6, when the light emission intensity output from the detector 12 is 10 or more when the rotation angle of the diffraction grating 111 is 10 degrees, it is determined that Fe is contained in the sample. The CPU 81 displays the qualitative elements on the display unit 84 by qualitative analysis performed in advance. From these displayed elements, the user selects a monitor element from the input unit 83. The CPU 81 accepts the input of the selected element, and when the temporal change in the emission intensity of the monitor element is larger than the predetermined value, it is determined whether the temporal change is within the predetermined range, or the emission intensity is It is determined whether or not it is greater than the comparative light emission intensity read from the qualitative analysis file 851, and the above-described measurement timing and cleaning end timing determination processing is performed. An element such as yttrium or a rare earth element having a predetermined concentration may be added to the sample, and the emission intensity of the added element may be measured. In this case, the CPU 81 receives information on the additive element input from the input unit 83, and the spectroscope control unit 112 rotates the diffraction grating 111 to an angle related to the additive element. Then, the above-described determination process of the measurement time and the cleaning end time is performed.

  The third embodiment is configured as described above, and the other configurations and operations are the same as those of the first and second embodiments. Therefore, corresponding parts are denoted by the same reference numerals, and detailed description thereof is omitted. To do.

Embodiment 4
FIG. 7 is a block diagram showing a hardware configuration of the ICP emission spectrometer 1 according to the fourth embodiment. The program for operating the ICP emission analysis apparatus 1 according to the first to third embodiments can be provided on a portable recording medium 1A such as a CD-ROM or a memory card as in the fourth embodiment. is there. Furthermore, the program can be downloaded from a server computer (not shown) via a communication network (not shown) such as a LAN or the Internet. The contents will be described below.

  A portable type recording program that allows a recording medium reader (not shown) of the ICP emission analyzer 1 shown in FIG. 7 to accept element selection, acquire emission intensity, determine the measurement time, and determine the cleaning end time. The recording medium 1A is inserted, and this program is installed in the program of the storage unit 85. Alternatively, such a program may be downloaded from an external server computer (not shown) via a communication unit (not shown) and installed in the storage unit 85. Such a program is loaded into the RAM 82 and executed. Thereby, it functions as the ICP emission analysis apparatus 1 of the present invention as described above.

  The fourth embodiment is configured as described above, and the other configurations and operations are the same as those of the first to third embodiments. Therefore, the corresponding parts are denoted by the same reference numerals and detailed description thereof is omitted. To do.

It is a block diagram which shows the hardware constitutions of the ICP emission analysis apparatus which concerns on this invention. It is a graph which shows the time change of the emitted light intensity output from a detector. It is a flowchart which shows the discrimination | determination process of a measurement time and washing | cleaning completion time. 10 is a flowchart showing a determination process of a measurement time and a cleaning end time according to the second embodiment. 6 is a block diagram showing a hardware configuration of an ICP emission analyzer according to Embodiment 3. FIG. It is explanatory drawing which shows the record layout of a qualitative analysis file. FIG. 10 is a block diagram showing a hardware configuration of an ICP emission analyzer according to a fourth embodiment.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ICP emission analyzer 8 Central control part 10 Introducing pipe 11 Spectrometer 12 Detector 13 Distilled water container 14 Sample container 81 CPU (control part)
82 RAM
83 Input unit 84 Display unit 85 Storage unit 851 Qualitative analysis file 111 Diffraction grating 112 Spectrometer control unit 1A Portable recording medium

Claims (13)

In a measurement timing discrimination method for discriminating the measurement timing of a sample by an ICP emission spectrometer that measures the emission intensity of an element in the sample,
A reception step for receiving an input of an element to be monitored;
An acquisition step of acquiring emission intensity relating to the element received in the reception step;
And a determination step for determining the measurement time of the sample based on the emission intensity acquired in the acquisition step. The end timing determination step of determining the cleaning end timing of the sample based on the emission intensity acquired by the acquisition step after the determination timing of the sample by the determination step is further provided. Method of determining the measurement time. The determination step includes
A change determining step for determining whether or not a temporal change in the emission intensity acquired by the acquiring step is greater than a predetermined value;
A range determining step for determining whether or not the temporal change in the emission intensity acquired by the acquiring step is within a predetermined range when the change determining step determines that the predetermined value is greater than the predetermined value;
The method according to claim 1, further comprising a step of discriminating that it is the measurement time of the sample when it is discriminated that it is within the predetermined range by the range discriminating step. The end time determination step includes
After determining the measurement time of the sample by the determination step, determining whether the temporal change in the emission intensity acquired by the acquisition step is greater than a predetermined value;
A step of determining whether or not the temporal change in the emission intensity acquired by the acquisition step is within a predetermined range when it is determined that the step is greater than the predetermined value;
The method according to claim 2 or 3, further comprising a step of discriminating that it is the cleaning end timing of the sample when it is discriminated within the predetermined range by the step. Before receiving the input of the element to be monitored by the receiving step, further comprising an analysis step of analyzing the composition of the sample based on the emission intensity corresponding to each element output from the spectrometer,
The receiving step includes
5. The measurement timing determination method according to claim 1, wherein an element in the sample analyzed by the analysis step is received as an element to be monitored. A step of adding an element other than the measurement target when the contained element of the sample is unknown,
The receiving step includes
The measurement time determination method according to any one of claims 1 to 5, wherein the added element is received as an element to be monitored. In an ICP emission spectrometer that measures the emission intensity of an element in a sample,
Receiving means for receiving input of elements to be monitored;
Obtaining means for obtaining the emission intensity of the element received by the receiving means;
An ICP emission analyzer comprising: a discriminating unit that discriminates a measurement timing of the sample based on the emission intensity acquired by the acquiring unit. 8. The apparatus according to claim 7, further comprising: an end time determination unit that determines a cleaning end time of the sample based on the emission intensity acquired by the acquisition unit after the determination unit determines the measurement time of the sample. ICP emission analyzer. The discrimination means includes
Change determination means for determining whether or not the temporal change in the emission intensity acquired by the acquisition means is greater than a predetermined value;
A range discriminating unit for discriminating whether or not the temporal change in the emission intensity acquired by the acquiring unit is within a predetermined range when it is determined by the change determining unit that the value is larger than the predetermined value;
9. The ICP emission analysis apparatus according to claim 7 or 8, further comprising means for discriminating that it is time to measure a sample when the range discriminating means discriminates that it is within a predetermined range. The end time determination means includes
Means for determining whether or not a temporal change in emission intensity acquired by the acquisition means is greater than a predetermined value after determining the measurement time of the sample by the determination means;
Means for determining whether or not the temporal change in the emission intensity acquired by the acquisition means is within a predetermined range when the means determines that the value is greater than the predetermined value;
The ICP emission analysis apparatus according to claim 8 or 9, further comprising means for discriminating that it is the cleaning end time of the sample when it is discriminated within the predetermined range by the means. Before receiving the input of the element to be monitored by the receiving means, further comprising analysis means for analyzing the composition of the sample based on the emission intensity corresponding to each element output from the spectrometer,
The accepting means is
The ICP emission analysis apparatus according to any one of claims 7 to 10, wherein an element in the sample analyzed by the analyzing means is received as an element to be monitored. In a program for discriminating the measurement time of a sample by an ICP emission spectrometer that measures the emission intensity of an element in the sample,
ICP emission analyzer
A reception step for receiving an input of an element to be monitored;
An acquisition step of acquiring emission intensity relating to the element received in the reception step;
And a determination step of determining a measurement time of the sample based on the emission intensity acquired in the acquisition step. 13. The process according to claim 12, further comprising: an end time determination step of determining a cleaning end time of the sample based on the emission intensity acquired in the acquisition step after determining the measurement time of the sample in the determination step. The program described.

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