JP2008298603A - Atomic absorption spectrometry and atomic absorption spectrophotometer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a heating temperature program, capable of calculating optimum heating time for a stage of drying and a stage of ashing of a sample, without having to depend on the experience of an analyst, and capable of obtaining optimum measurement with accuracy through minimum times of measurement. <P>SOLUTION: The atomic absorption spectrometry and atomic absorption spectro-photometer is provided with a step for heating and atomizing the measurement sample; a step for radiating measurement light to the atomized sample; a step for dispersing the measurement light passing through the heating step for each arbitrary wavelength, a step for detecting the light dispersed by the light-dispersing step; a step for calculating the absorbance from a signal output by the detection step; a step for inputting the heating temperature and the time of the heating step; a step for storing an absorbance determination value; a step for comparing and determining between the value of the absorbance obtained in an arbitrary period in heating of a preceding stage for atomizing and measuring the measurement sample and the stored absorbance determination value; and a step for calculating the heating time of the measurement sample of the preceding stage, from the result of the comparison and determination treatment. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to an atomic absorption analysis method and an atomic absorption spectrophotometer, and in particular, in a pre-measurement stage of a measurement sample that is a liquid, water is evaporated in a dry heating stage, and then in an ashing heating stage, organic substances are combusted and ashed. The present invention relates to an atomic absorption analysis method and an atomic absorption spectrophotometer in which a metal element is analyzed by performing atomization in an atomization heating stage and performing an absorption analysis of the atomic vapor.

  Electric furnace analysis atomic absorption spectrophotometer injects several μL to several tens of μL of a liquid measurement sample into a graphite tube, and evaporates the moisture in the measurement sample, and burns and ashes organic substances. Then, analysis is performed by heating to a temperature at which the measurement sample is finally atomized. The drying temperature and time, ashing temperature and time, atomization temperature and time are determined by the analyst according to the sample injection amount, sample component, and analysis element based on experience, and input to the controller as a heating temperature program for analysis. .

  In addition, after measurement, the reproducibility and analysis sensitivity of the measurement data are confirmed, and the temperature and time are changed at the discretion of the analyst, and analysis is performed again. By repeating the above, the target reproducibility and analytical sensitivity are obtained.

JP-A-6-94606 JP-A-11-21657 JP 2001-83082 A JP 2005-308681 A

  However, as with the prior art, it is necessary to repeat the analysis work of the analyst and the measurement data, so that only non-experienced persons can perform the analysis, and the time to repeat the analysis until good reproducibility and analytical sensitivity are obtained. Was necessary.

  When the amount of the injected sample is 20 μL, the drying is set at about 80 ° C. to 140 ° C. and the heating time is usually set at about 30 to 50 seconds, but strictly speaking, the time until the sample is dried may be a little shorter. Moreover, when the sample amount is increased, it is necessary to increase the time. However, if the sample proceeds to the ashing stage before drying, the moisture before evaporation evaporates and scatters in the graphite tube, causing the problem of reduced measurement reproducibility and absorption sensitivity. Set for a long time with. In the case of ashing, it varies depending on the element to be measured, and the heating time is usually set to about 20 to 40 seconds at about 400 ° C to 1000 ° C. In addition, when the sample amount is increased, it is necessary to lengthen the time.

  However, if the sample is not completely incinerated and the process proceeds to the atomization stage, there is a problem that the amount of background (smoke) generated during atomization increases and the accuracy of the analysis decreases. It is set to a long time with a margin.

  Based on the above, it is necessary to repeat the measurement several times while changing the experience and time of the analyst to set the heating temperature program in the drying stage and the ashing stage, and the measurement accuracy is good depending on the level of the experience value of the analyst. Defects are affected, the determination of drying time or ashing time is made indirectly by looking at the measurement reproducibility or absorption sensitivity, and what measurement takes 2 to 4 minutes per measurement I had to repeat it again.

  The object of the present invention is to obtain the optimum heating time in the drying and ashing stages without depending on the experience of the analyst, and to achieve the optimum measurement accuracy with the minimum number of measurements without repeating the measurement many times. It is to realize an atomic absorption photometer capable of obtaining the obtained heating temperature program.

  The present invention includes a heating step for heating and atomizing a measurement sample, a light emission step for irradiating measurement light to the atomized sample, and spectroscopy for spectroscopically analyzing the measurement light that has passed through the heating step for each arbitrary wavelength. A detection step for detecting light separated by the spectroscopic step, a calculation step for calculating the absorbance from the signal output by the detection step, an input step for instructing and inputting the heating temperature and time of the heating step, and the absorbance A storage step for storing a determination value, and further comparing and determining the absorbance value obtained in an arbitrary period during heating before the measurement sample is atomized and measured, and the stored absorbance determination value A pre-stage process including a step of performing and a step of obtaining a measurement sample heating time of the pre-stage to be atomized and measured from the result of the comparison determination process There is provided an atomic absorption spectrometry, wherein.

  Further, the present invention provides a heating means for heating and atomizing a measurement sample, a light emitting means for irradiating measurement light to the atomized sample, and measuring light passing through the heating means for each wavelength. Spectroscopic means, detecting means for detecting the light split by the spectroscopic means, computing means for calculating the absorbance from the signal output by the detecting means, and input for instructing the heating temperature and time of the graphite tube And a control means for controlling each of the means, and the control means is obtained in an arbitrary period during heating in the previous stage of measuring the measurement sample by atomizing the measurement sample, and storing the absorbance determination value. A comparison / determination unit that compares and determines the absorbance value obtained and the absorbance determination value of the storage unit; and a time calculation unit that calculates a measurement sample heating time in a previous stage for measurement by atomization from the result of the comparison determination process; Have There is provided an atomic absorption spectrophotometer according to claim.

  According to the present invention, the optimum heating time for the drying and ashing stages of the sample is obtained without depending on the experience of the analyst, and the optimum measurement is performed with the minimum number of measurements without repeating the measurement over and over. It is possible to realize an atomic absorption photometer capable of obtaining a heating temperature program capable of obtaining accuracy.

  Examples of the embodiment of the present invention are as follows.

  In the atomic absorption analysis method, the absorbance value obtained in an arbitrary period during heating before the measurement sample is atomized and measured is compared with a preset first determination value, and the absorbance value is determined. A first step for detecting that the absorbance has increased; the absorbance value obtained during an arbitrary period during the heating after the detection is compared with a preset second determination value, and the absorbance value has decreased There is provided an atomic absorption analysis method characterized by having a second step of detecting the temperature and a third step of recording the accumulated accumulated time. The measurement sample is generally heated in the graphite tube, and the same applies to the embodiment of the present invention.

  A heating step for heating and atomizing the measurement sample; a light emission step for irradiating the atomized sample with measurement light; and a spectroscopic step for splitting the measurement light that has passed through the heating means for each arbitrary wavelength. , Separating the light dispersed by the spectroscopic means into light having a deflection component parallel to the magnetic field and light having a component perpendicular to the magnetic field, and detecting each light, and parallel to the magnetic field output by the detection step An atomic absorption analysis method comprising: a calculation step for calculating each absorbance from a signal of a vertical deflection component and a signal of a vertical component; and an input step for indicating and inputting a heating temperature and time. The absorbance value of the component perpendicular to the magnetic field obtained during an arbitrary period during the heating before the measurement is compared with the first determination value set in advance to detect that the absorbance value has increased. 1 and comparing the absorbance value of the component perpendicular to the magnetic field obtained in the arbitrary period during the heating after the detection with a preset second determination value, and detecting that the absorbance value has decreased There is provided an atomic absorption analysis method characterized in that the method has a second step and a third step of recording the accumulated accumulated time.

  In the above method, any one of a first case in which the first to third steps are performed only in the drying stage, a second case in which only the ashing stage is performed, and a third case in which both the drying stage and the ashing stage are performed. Can be included. Further, in the above method, the heating is terminated after a preset time from when the decrease in the absorbance value is confirmed in the second step, and the process proceeds to the next heating stage or the atomization stage for performing the measurement. Can do. Further, in the method, the drying stage and the ashing stage can be set to a plurality of stages.

  Further, it is a method for performing atomic absorption analysis using an atomic absorption photometer equipped with a deuterium discharge tube for background detection in addition to measurement light, wherein the measurement sample is atomized and measured before the measurement. A step of comparing and determining the absorbance value of the deuterium discharge tube obtained during an arbitrary period during heating and the absorbance determination value of the storage means; Determining a measurement sample heating time.

  The present invention comprises a heating means having a graphite tube for heating and atomizing a measurement sample, a light emitting means for irradiating measurement light to the atomized sample, and measurement light having passed through the heating means for any wavelength. Spectroscopic means for spectrally separating the light, detection means for detecting the light dispersed by the spectral means, calculation means for calculating the absorbance from the signal output by the detection means, and the heating temperature and time of the graphite tube are input as instructions And a control means for controlling each of the means, the control means presetting the absorbance value obtained in an arbitrary period during heating before the measurement sample is atomized and measured. A first means for detecting an increase in the absorbance value compared to the first determination value, and an absorbance value obtained in an arbitrary period during the heating after the detection and a preset first value. Compared with the judgment value of 2, Second means for detecting that the value of the degree drops, provides an atomic absorption spectrophotometer and a third means for recording heated cumulative time.

  Also, a heating means having a graphite tube arranged in a DC magnetic field for heating and atomizing the measurement sample, a light emitting means for irradiating the atomized sample with measurement light, and measurement passing through the heating means Spectroscopic means for splitting light at an arbitrary wavelength, and separating the light split by the spectral means into light having a deflection component parallel to the magnetic field and light having a component perpendicular to the magnetic field, and detecting each light Detecting means, calculating means for calculating each absorbance from a signal of a component perpendicular to the deflection component signal parallel to the magnetic field output by the detecting means, and the heating temperature and time of the graphite tube are instructed. Input means and control means for controlling each of the means, and the control means is an absorbance of a component perpendicular to a magnetic field obtained in an arbitrary period during heating before the measurement sample is atomized and measured. Value and preset number A first means for detecting an increase in the absorbance value, and an absorbance value of a component perpendicular to the magnetic field obtained in an arbitrary period during the heating after the detection. An atomic absorption photometer comprising: a second means for detecting that the absorbance value has decreased as compared with a second determination value; and a third means for recording the accumulated accumulated time. provide.

  In the apparatus, a first case in which the first to third means are performed only in the drying stage, a second case in which only the ashing stage is performed, and a third case in which both the drying stage and the ashing stage are performed. There can be means for selecting either. Further, the heating at that stage is terminated after a preset time from when the decrease in the absorbance value is confirmed by the second means, and the process proceeds to the next heating stage or the atomization stage where the measurement is performed. it can.

  Further, in the apparatus, the drying stage and the ashing stage can be set to a plurality of stages. In addition to the measurement light, a deuterium discharge tube for background detection is provided, and the absorbance value of the deuterium discharge tube obtained during an arbitrary period during heating before the measurement sample is atomized and measured. And means for comparing and determining the absorbance determination value of the storage means, and means for obtaining the measurement sample heating time in the previous stage of measurement by atomization from the result of the comparison determination process.

  As the absorbance value used for the above determination, the absorbance value varied depending on the background is used for the determination for the following reason. In the drying stage, the measurement light is blocked by the background of water vapor or the like generated when the moisture of the liquid measurement sample evaporates, and the absorbance is lowered. In the ashing stage, the measurement light is blocked by the background of smoke or the like generated when the organic matter or the like of the dried measurement sample is burned, and the absorbance decreases.

  Paying attention to this phenomenon, the state of drying and ashing can be judged by monitoring and detecting the change in absorbance due to the background of the drying and ashing stages, which is the heating before the measurement sample is atomized. To do.

  The objective of finding the optimal heating time for the drying and ashing stages was to obtain the minimum number of measurements by recording the absorbance during the drying and ashing stages and judging the background state. .

  Embodiments of the present invention will be described below with reference to examples and drawings.

  FIG. 1 is a schematic configuration diagram of an atomic absorption photometer according to a first embodiment of the present invention. In FIG. 1, measurement light 4 is irradiated from a light source 3 onto a sample 17 that is a measurement target injected into the graphite tube 2. The heating control unit 14 controls the heating of the electric heating furnace 1 according to the heating temperature program input and set in advance by the operation unit 12, the graphite tube 2 is energized and heated by the electric heating furnace 1, and the sample 17 is in the drying stage and ashed Atomized through stages.

  When the sample 17 is heated, a magnetic field is applied to the sample 17 by the DC magnetic circuit 5 of the electric heating furnace 1, so that light having a polarization component parallel to the magnetic field (referred to as sample light) is converted into an atomized metal element and water vapor. On the other hand, light of a polarized light component perpendicular to the magnetic field (referred to as reference light) is absorbed slightly by the atomized metal element and the background 18 of water vapor, smoke, etc. To be absorbed. For this reason, the detection of the background 18 such as water vapor and smoke generated from the sample 17 being heated is determined by monitoring fluctuations in the absorption of the vertically polarized component light (referred to as reference light) 16.

  The measurement light 4 that has passed through the sample 17 is guided to the spectrometer 6. The spectroscope 6 splits the measurement light 4, and only the light having a specific measurement wavelength to be measured is emitted from the spectroscope 6.

  The emitted measurement light 44 is separated by the polarizing prism 7 into a polarized light component 15 parallel to the magnetic field and a vertical polarized light component 16 at a separation angle of 4 °.

  Parallel polarized component light (referred to as sample light) 15 separated from each other is guided to a detector [photomultiplier tube (first detector)] 8, while vertical polarized component light (referred to as reference light) 16. Is guided to a detector (photomultiplier tube (second detector)) 9.

  The detector 8 and the detector 9 convert the light intensity into an electric signal and output it to the A / D converter 10. The A / D converter 10 outputs the electric signal as a digital signal to the central processing unit 11. The central processing unit 11 has a storage device 50 that calculates and stores absorbance from a digital signal, and outputs it to the operation unit 12 and displays it on the display unit 13.

  The central processing unit 11 continuously monitors the absorbance, and sets the absorbance value of the vertically polarized component light (referred to as reference light) 16 in advance during the heating before the measurement sample is atomized and measured. The first determination value (background detection start absorbance value) is compared with the first determination value, the absorbance value is increased and the background is detected, and the vertical obtained after the detection at any time during the heating Compare the absorbance value of the polarization component light (referred to as reference light) 16 with a preset second determination value (absorbance value at the end of background detection), and the second value at which the absorbance value falls and the detection of the background ends. Step 3 and a third step of recording the accumulated cumulative time are executed. FIG. 2 shows an example of the display unit 13 displaying the change in absorbance from the measurement sample drying stage to the ashing stage to atomization in real time.

  Therefore, in the present invention, the central processing unit 11 continuously monitors the change in absorbance due to the background and performs the determination process as shown in FIG. Note that a plurality of determination values are used in the determination process shown in FIG. 3, but each determination value is set in advance by an analyst. Table 1 shows an example of initial setting values and determination setting ranges of determination values. In the table, abs is the absorbance.

以下、図３の本発明によるバックグラウンドによる吸光度変化から乾燥段階および灰化段階の加熱時間を求める分析のフローチャートについて説明する。まず、分析者が予め分析条件の設定を行う。設定項目は、測定元素、測定波長であり、加熱温度プログラムにおいては、乾燥段階の開始温度、終了温度、加熱時間Ａ、灰化段階の開始温度、終了温度、加熱時間Ｂ、原子化段階の温度、加熱時間であり、バックグラウンド検出においては、乾燥段階の検出開始判定吸光度値Ｃ、検出終了判定吸光度値Ｄ、灰化段階の検出開始判定吸光度値Ｅ、検出終了判定吸光度値Ｆである。

Hereinafter, the analysis flowchart for obtaining the heating time in the drying stage and the ashing stage from the change in absorbance due to the background according to the present invention in FIG. 3 will be described. First, an analyst sets analysis conditions in advance. Setting items are measurement element and measurement wavelength. In the heating temperature program, the drying stage start temperature, end temperature, heating time A, ashing stage start temperature, end temperature, heating time B, atomization stage temperature In the background detection, the detection start determination absorbance value C, the detection end determination absorbance value D, the ashing stage detection start determination absorbance value E, and the detection end determination absorbance value F in the background detection.

  Next, the sample 17 is injected into the graphite tube 2 and the heating temperature program is started. The heating temperature program begins with a drying phase that evaporates the moisture in the sample.

  After the start of heating in the drying stage, a reference absorbance value is calculated in order to determine whether to start background detection. The reference absorbance value is an absorbance value calculated from the current light intensity detected by the detector 9 and the light intensity before heating. Then, the calculated reference absorbance value is compared with the “detection start determination absorbance value C” shown in Table 1. If the reference absorbance value is less than C, it is determined that the background has not been detected yet, and the process proceeds to the time-out determination process, and the cumulative drying time in the drying stage is compared with “heating time A” shown in Table 1. .

  If the dry heating cumulative time is less than A, it waits for 1,000 ms, and the background detection start determination process is performed again. When the reference absorbance value ≧ C, the process proceeds to the determination of the end of the next drying stage background detection. Moreover, when the dry heating cumulative time ≧ A, the drying stage is finished and the ashing stage is advanced. Note that the detection sensitivity can be freely adjusted by changing the setting of the detection determination value C.

  In the determination of the end of the drying stage background detection, the reference absorbance value is compared with the “detection end determination absorbance value D”. If the reference absorbance value is greater than or equal to D, it is determined that the background is still occurring, and the process proceeds to the time-out determination process, and the drying heating cumulative time in the drying stage is compared with the “heating time A”. If the dry heating cumulative time is less than A, the process waits for 1,000 ms, and performs the background detection end determination process again.

  When the reference absorbance value <D, after 5,000 ms has elapsed, the drying stage is terminated and the process proceeds to the next ashing stage. Moreover, when the dry heating cumulative time ≧ A, the drying stage is finished and the ashing stage is advanced. In synchronization with this execution, the accumulated time of the drying stage is recorded. The detection end sensitivity can be freely adjusted by changing the setting of the detection determination value D. The next step after 5,000 ms elapses is to add time in consideration of the variation in drying completion for each measurement.

  Next, the reference absorbance value is compared with the “detection start determination absorbance value E” in order to determine whether background detection starts after the start of heating in the ashing stage in which the organic matter or the like of the sample is combusted. If the reference absorbance value is less than E, it is determined that the background has not been detected yet, and the process proceeds to the time-out determination process, and the ashing heating cumulative time in the ashing stage is compared with the “heating time B”. If the accumulated ashing time is less than B, the process waits for 1,000 ms, and the background detection start determination process is performed again.

  If the reference absorbance value ≧ E, the process proceeds to the next ashing stage background detection end determination. Moreover, when the ashing heating cumulative time ≧ B, the ashing stage is terminated and the atomization stage is advanced. Note that the detection sensitivity can be freely adjusted by changing the setting of the detection determination value E.

  In the determination of the end of the ashing stage background detection, the reference absorbance value is compared with the “detection end determination absorbance value F”. If the reference absorbance value is F or more, it is determined that the background is still occurring, and the process proceeds to the time-out determination process, and the accumulated ashing heating time in the ashing stage is compared with the “heating time B”. If the accumulated ashing time is less than B, the process waits for 1,000 ms, and the background detection end determination process is performed again.

  When the reference absorbance value <F, after the lapse of 5,000 ms, the ashing stage is finished and the process proceeds to the next atomization stage. Moreover, when the ashing heating cumulative time ≧ B, the ashing stage is terminated and the atomization stage is advanced. In synchronization with this execution, the accumulated time of the ashing stage is recorded. Note that the detection end sensitivity can be freely adjusted by changing the setting of the detection determination value F. The reason why the process proceeds to the next after the lapse of 5,000 ms is that the time is added in consideration of variations in ashing completion for each measurement.

  Next, in the atomization stage, the measurement of taking in the absorbance during the heating time (measurement time) G is performed. After the measurement, the accumulated time of each heating in the drying stage and the ashing stage is reflected in the drying stage heating time A and the ashing stage heating time B of the analysis conditions.

  As described above, according to the first embodiment of the present invention, by detecting the change in absorbance due to the background of the drying stage and the ashing stage, which is heating before the measurement sample is atomized and measured, In the drying stage, the start of water vapor generation and the end time of water vapor generation can be recorded.

  In addition, at the ashing stage, it is possible to record the start time of smoke generation and the end time of smoke generation due to combustion of organic matter or the like. By reflecting this recorded time in the heating temperature program, it is possible to perform measurement with the optimum and shortest heating time that allows sufficient drying and ashing. Therefore, the optimum measurement accuracy can be obtained with the minimum number of measurements without depending on the experience of the analyst.

It is a schematic block diagram of the atomic absorption photometer by embodiment of this invention. It is an example of the display part which displays the light-absorbency change from the drying stage of a measurement sample to an ashing stage and atomization in real time. It is a flowchart of the analysis which calculates | requires the heating time of a drying stage and an ashing stage from the light absorbency change by the background by this invention.

Explanation of symbols

  DESCRIPTION OF SYMBOLS 1 ... Electric heating furnace, 2 ... Graphite tube, 3 ... Light source, 4 ... Measuring light, 5 ... DC magnetic circuit, 6 ... Spectroscope, 7 ... Polarizing prism, 8 ... Detector (photomultiplier tube), 9 ... Detection (Photomultiplier tube), 10 ... A / D converter, 11 ... central processing unit, 12 ... operation unit, 13 ... display unit, 14 ... heating control unit, 15 ... parallel polarized component light (referred to as sample light) 16 ... Vertically polarized component light (referred to as reference light), 17 ... Sample, 18 ... Background (water vapor, smoke), 44 ... Measuring light, 50 ... Storage device.

Claims (14)

  A heating step for heating and atomizing the measurement sample, a light emission step for irradiating the atomized sample with measurement light, a spectroscopic step for splitting the measurement light that has passed through the heating step for each arbitrary wavelength, A detection step for detecting the light separated by the step, a calculation step for calculating the absorbance from the signal output by the detection step, an input step for instructing input of the heating temperature and time of the heating step, and an absorbance determination value are stored. And a step of comparing and comparing the absorbance value obtained during an arbitrary period during the heating before the measurement sample is atomized and the stored absorbance determination value; A pre-stage process including a step of obtaining a heating time of a measurement sample of a pre-stage to be atomized and measured from a result of the comparison determination process; Atomic absorption spectrometry that.   In the atomic absorption analysis method according to claim 1, comparing the absorbance value obtained during an arbitrary period during the heating before the measurement sample is atomized and measured with a first determination value set in advance, A first step of detecting an increase in the absorbance value, a comparison between the absorbance value obtained in the optional period during the heating after the detection and a preset second determination value, and the absorbance value; An atomic absorption analysis method comprising: a second step for detecting that the temperature has decreased; and a third step for recording the accumulated cumulative time.   A heating step for heating and atomizing the measurement sample, a light emission step for irradiating the atomized sample with measurement light, a spectroscopic step for splitting the measurement light that has passed through the heating step for each arbitrary wavelength, The light separated by the step is separated into light having a deflection component parallel to the magnetic field and light having a component perpendicular to the magnetic field, and a detection step for detecting each light, and deflection parallel to the magnetic field output by the detection step An atomic absorption analysis method comprising: a calculation step for calculating each absorbance from a component signal perpendicular to a component signal; and an input step for instructing and inputting the heating temperature and time, and further atomizing the measurement sample Compare the absorbance value of the component perpendicular to the magnetic field obtained during an arbitrary period during heating in the previous stage of measurement with the first judgment value set in advance, and check that the absorbance value has increased. Comparing the absorbance value of the component perpendicular to the magnetic field obtained in the arbitrary period during the heating after the detection with the second determination value set in advance, and the absorbance value has decreased An atomic absorption analysis method, comprising: a second step of detecting the temperature, and a third step of recording the accumulated cumulative time of heating.   A step of selecting any one of the first case in which the first to third steps are performed only in the drying stage, the second case in which only the ashing stage is performed, and the third case in which both the drying stage and the ashing stage are performed. The atomic absorption analysis method according to claim 3, wherein   The heating at this stage is terminated after a preset time from when the decrease in absorbance value is confirmed in the second step, and the process proceeds to the next heating stage or the atomization stage where measurement is performed. The atomic absorption analysis method according to claim 4.   6. The atomic absorption analysis method according to claim 5, wherein the drying stage and the ashing stage are set to a plurality of stages.   A method of performing atomic absorption analysis using an atomic absorption photometer equipped with a deuterium discharge tube for background detection in addition to measurement light, wherein the measurement sample is atomized and measured before heating A step of performing comparison determination between the absorbance value of the deuterium discharge tube obtained during an arbitrary period of time and the stored absorbance determination value, and heating the measurement sample at the previous stage for atomization and measurement from the result of the comparison determination process The atomic absorption analysis method according to claim 1, further comprising a step of obtaining time.   A heating means for heating and atomizing the measurement sample; a light emitting means for irradiating the atomized sample with measurement light; a spectroscopic means for splitting the measurement light that has passed through the heating means for each arbitrary wavelength; and Control means for detecting light split by the spectroscopic means, calculating means for calculating absorbance from the signal output from the detecting means, input means for inputting the heating temperature and time, and controlling each of the means Control means, the control means for storing the absorbance determination value, the absorbance value obtained in an arbitrary period during heating before the measurement sample is atomized and measured, and the storage means Atomic absorption spectrophotometer characterized by having a comparison / determination function for comparing and determining with an absorbance determination value and a time calculation function for obtaining a measurement sample heating time at the previous stage of measurement by atomizing from the result of the comparison determination process Total   A heating means for heating and atomizing the measurement sample; a light emitting means for irradiating the atomized sample with measurement light; a spectroscopic means for splitting the measurement light passing through the heating means for each arbitrary wavelength; Control means for detecting the light dispersed by the means, calculation means for calculating the absorbance from the signal output by the detection means, input means for inputting the heating temperature and time, and controlling each means A control means, and the control means compares the absorbance value obtained during an arbitrary period during heating before the measurement sample is atomized and measured with a first determination value set in advance, A first means for detecting that the absorbance value has increased, a comparison between the absorbance value obtained in the arbitrary period during the heating after the detection and a preset second determination value; Second to detect that has fallen Atomic absorption spectrophotometer, characterized in that it comprises a third means for performing a unit, the recording of the heated cumulative time.   A heating means arranged in a DC magnetic field for heating and atomizing the measurement sample, a light emitting means for irradiating the atomized sample with measurement light, and the measurement light passing through the heating means for each arbitrary wavelength Spectroscopic means for separating the light, light separated by the spectroscopic means into light having a deflection component parallel to the magnetic field and light having a component perpendicular to the magnetic field, and detecting means for detecting each light, and the detection Control means for calculating the respective absorbances from the signals of the deflection component and the component perpendicular to the magnetic field output by the means, the input means for inputting the heating temperature and time, and controlling the means A control means, wherein the control means comprises an absorbance value of a component perpendicular to the magnetic field obtained in an arbitrary period during heating before the measurement sample is atomized and measured, and a preset first determination value The absorbance value is higher than Comparing the absorbance value of the component perpendicular to the magnetic field obtained in the arbitrary period during the heating after the detection with a second determination value set in advance, An atomic absorption photometer comprising: a second means for detecting that the value has decreased; and a third means for recording the accumulated cumulative time.   11. The first case in which the first to third means are performed only in the drying stage, the second case in which only the ashing stage is performed, and the third case in which both the drying stage and the ashing stage are performed. An atomic absorption photometer comprising selection means for selecting any of the above.   In Claim 11, the said selection means complete | finishes heating after the preset time from when the fall of the value of the absorbance was confirmed by the 2nd means, and the atomization stage which performs a next heating stage or a measurement An atomic absorption photometer characterized in that the step of proceeding to is executed.   The atomic absorption photometer according to claim 12, wherein the selection means has a function of setting a drying stage and an ashing stage to a plurality of stages.   11. The method according to claim 8, further comprising a deuterium discharge tube for detecting a background in addition to the measurement light, and obtained during an arbitrary period during heating before the measurement sample is atomized and measured. Means for making a comparison between the absorbance value of the deuterium discharge tube and the absorbance judgment value of the storage means, means for obtaining the measurement sample heating time in the previous stage of measurement by atomizing from the result of the comparison judgment process; An atomic absorption photometer characterized by comprising:

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