JP5949613B2 - Spectrophotometer - Google Patents

Description

  The present invention relates to a spectrophotometer having a function of diagnosing power spectrum intensity when an apparatus is initialized.

  In general, in a spectrophotometer such as FTIR, the signal intensity (background signal) when the sample is not placed on the photometric optical path and the signal intensity (sample signal) when the sample is placed on the photometric optical path. By obtaining the ratio (division) by the wave number width (or wavelength width) within a preset range, an absorption spectrum by the sample itself is obtained. In order to obtain a good absorption spectrum at this time, it is necessary that the amount of detection light emitted from the light source, transmitted through the sample and incident on the detector is more than a certain level, and can be detected with a sufficiently large signal intensity. It is.

  In order to obtain a signal intensity necessary to obtain a good absorption spectrum, it is necessary that all of the intensity of light emitted from the light source, the sensitivity of the detector, and the optical axis adjustment of the optical system are good. For this reason, in FTIR, etc., conventionally, when the apparatus is initialized, the optical system including the measurement of the power spectrum intensity is self-diagnosed so that the apparatus can measure with sufficient signal intensity. Are inspected (see Non-Patent Document 1).

For example, FIG. 4 is a schematic diagram showing measurement data of power spectrum intensity measured for inspection of the optical system at the time of initialization in FTIR.
The measurement data of the power spectrum intensity is obtained by measuring the signal corresponding to the preset wave number range so that the measurement light (infrared light) emitted from the light source is incident on the detector without passing through the sample. The In FTIR, a power spectrum is obtained by Fourier transforming an interferogram of interference light detected without passing through a sample.

For inspection, specific wave numbers (for example, 3000 cm ⁻¹ , 2000 cm ⁻¹ , 1000 cm ⁻¹ ) are selected as standard wave numbers, and standard values A, B, and C at these standard wave numbers are set in advance. The standard value is a value determined by the combination of the detector and the light source to be used, and is a value that can guarantee that normal measurement can be performed if the standard value or more.

In the self-diagnosis of the power spectrum at the time of initialization, the measured value and the standard value are compared at these three specific wave numbers to determine whether or not it is in a normal state.
As a result of self-diagnosis, as shown in FIG. 4 (a), when measured data of power spectrum intensity exceeding the standard value is obtained for all three points, the diagnostic test result is passed, as shown in FIG. Otherwise, the test result is rejected when measurement data is obtained.

A screen display example of the diagnosis result is shown in FIG. Here, a standard value, an actual measurement value, and a determination result (indicating that “good” is good) at specific wave numbers (3000 cm ⁻¹ , 2000 cm ⁻¹ , 1000 cm ⁻¹ ) are displayed.
Based on the determination result, the measurer continues the measurement when the determination is acceptable, and performs maintenance work for adjustment when the determination is failure.
It should be noted that the numerical value used as a criterion for determining whether or not the power spectrum intensity is acceptable may be other than the signal intensity of the three specific wave numbers described above. For example, the average value until the previous measurement may be used as a reference, or the maximum photometric value within the measurement wavenumber range may be used as a reference.

Shimadzu Home Page> Product Information> Optical Analysis (Spectro Instruments)> Fourier Transform Spectrophotometer (FT-IR)> IRsolution [online], Internet <URL; http://www.an.shimadzu.co.jp/ftir/ irsol / irsol.htm>

If a pass determination is given in the power spectrum intensity test at the time of initialization, stable measurement is guaranteed.
However, the pass / fail judgment is a method of judging by comparing the measured value of the power spectrum intensity with the standard value, so if it exceeds the standard value, it will pass, so unless the measurer carefully records the light source And the degree of progress and stability of the detector could not be grasped.

  In FTIR, a ceramic heater is used as a light source and a TGS detector is used as a detector, and these parts may suddenly become defective. It is thought that it often deteriorates little by little.

  In view of this, the present invention enhances the diagnosis based on the test of the power spectrum intensity so that it can predict the time when it will be judged as rejected. For example, it is possible to predict the replacement time and maintenance time of parts early. The purpose is to provide a photometer.

The spectrophotometer of the present invention, which has been made to solve the above-mentioned problems, is a measured value of the power spectrum intensity obtained from the detection signal measured in a state where the light emitted from the light source is incident on the detector without passing through the sample. the power spectrum intensity measurement test for comparing with a preset standard value of the power spectral intensity, a spectrophotometer equipped with a power spectrum diagnostic unit to run when initializing the at least spectrophotometer the power A history information storage control unit that stores an actual value of spectrum intensity as history information together with date and time information on which the detection was performed, and a history information display control unit that displays history information when receiving a display request signal , The history information display control unit, when a new power spectrum intensity measurement test is executed, In addition, the previous actual measurement value, the average value up to the previous time, or the reference value obtained by performing the calculation process using the history information is displayed side by side, and the history is further displayed. An editing function for deleting a part of the history information can be executed for the history information stored by the information storage control unit, and whether or not the history information can be used in the calculation process without deleting the part of the history information. A history information editing control unit capable of executing an editing function for selecting settings is provided .

  According to the present invention, the power spectrum diagnostic unit executes a power spectrum intensity measurement test at the time of initialization, compares the measured value with a pre-stored standard value, and determines whether the apparatus can be stably measured. The diagnosis result is displayed. In addition, the history information storage control unit stores the actual measurement value of the power spectrum intensity measurement test as history information in association with the date and time information on which the measurement was performed. Therefore, the history information display control unit always displays history information including date and time information and measured values on the screen by receiving input of the measurer and a display request signal at the time set in advance by the program. It is possible to refer to the transition of the value, which can be useful for predicting the replacement timing of the light source and the detector and the timing when the optical axis maintenance is necessary.

In addition , when a new power spectrum intensity measurement test is executed, the history information display control unit, together with the newly detected power spectrum intensity actual measurement value, the previous actual measurement value, the average value until the previous time, or the history information the operator displays side by side either history reference value reference value obtained by arithmetic processing using.
Therefore, the current actual measurement value and the past historical reference value are compared by displaying the historical actual measurement value, the average value, and the history reference value (which may be a plurality) of the reference values side by side. This makes it easier to predict the time for lamp replacement and maintenance.

Et al is, the history information stored by the history information storage control unit, it is possible to perform editing functions to remove a portion of the history information, together with the operation without deleting the part of the history information so that it includes history information editing control unit capable of performing the editing function of selecting whether setting of the use of the process.
Therefore , history information, etc., when the photometric value is abnormal due to obvious erroneous measurement, can be deleted from the history information when calculating the average value or calculating the reference value, and is not subject to calculation. You can also Conversely, it can also be used for calculation again .

  In the above invention, the spectrophotometer includes an accessory sensor that detects whether or not a measurement accessory is attached, and an accessory confirmation unit that checks the presence or absence of the measurement accessory based on a signal from the accessory sensor. The information editing control unit deletes the power spectrum intensity measurement test when the accessory confirmation unit confirms the attachment of the measurement accessory so that it is not included in the history information, or removes it from use in the editing function. In this way, the editing function may be executed.

  When a measurement accessory is attached, the signal is weakened due to the effect, so adding it to the history information makes it inconsistent with other history information, so the attachment state is automatically detected by the accessory sensor and is not subject to computation. By doing so, the data of the measurement test when the accessory is mounted can be reliably excluded from the calculation when calculating the average value or the reference value.

The block block diagram which shows schematic structure of FTIR which is one Embodiment of this invention. The figure which shows the example of a screen display of the power spectrum intensity | strength measurement result in FTIR of FIG. The figure which shows the example of a screen display at the time of displaying the list | wrist of the accumulated history information. The schematic diagram which shows the measurement data of the power spectrum intensity | strength measured at the time of initialization. The figure which showed the example of a screen display of the conventional power spectrum intensity | strength measurement result.

  The present invention will be described below with reference to the drawings. FIG. 1 is a block diagram showing a schematic configuration of FTIR which is an embodiment of the present invention.

The FTIR 10 includes an infrared light source 11, a photometric optical system 14 including an interferometer 12 and a measurement chamber 13, a detector 15, and a control unit 20 that controls them.
A ceramic light source is used as the light source 11. An optional tungsten iodine lamp is mounted for near infrared measurement.
As the interferometer 12, a Michelson interferometer including a moving mirror, a fixed mirror, and a beam splitter is used, and the moving mirror is driven to form interference light. In addition, the measurement chamber 13 is provided in the subsequent stage of the interferometer 12 so that interference light is irradiated to a sample disposed on the photometric light path in the measurement chamber 13.

  Although not shown in the photometric optical system 14, in addition to the interferometer 12 and the measurement chamber 13, a collimator mirror and an interferometer 12 that send the measurement light from the infrared light source 11 to the interferometer 12 as a parallel beam. Some condensing mirrors that collect measurement light (interference light) emitted from the sample at the sample installation position in the measurement chamber 13 and some detection condensing mirrors that guide the measurement light that has passed through the sample installation position to the detector 15 The optical parts are also included.

  The measurement chamber 13 is provided with an accessory sensor 13a that detects whether or not a measurement accessory is attached. The measurement accessories include, for example, an total reflection measurement device (ATR), a diffuse reflection measurement device, and the like. When these are attached to the measurement chamber 13, the accessory sensor 13a (for example, a mechanical switch) is activated to indicate that it is in a mounted state. A detection signal is output. The presence / absence of a detection signal from this sensor is detected by an accessory confirmation unit 35 described later.

  A TGS detector is used as the detector 15. If an optional MCT detector (mid-infrared) or InGaAs detector (near-infrared) is attached separately from the TGS detector, one of the detectors is rotated by the rotation of the above-described condensing mirror for detection. The optical path is switched so that the measurement light is incident on the optical path.

  In the following, for convenience of explanation, it is assumed that a ceramic light source is used as the light source 11 and a TGS detector is used as the detector 14 at the time of initialization of the apparatus, but initialization is performed with other combinations of light sources and detectors. Is performed, the standard value (set value) of the pass / fail judgment is changed.

  Next, the control unit will be described. The FTIR 10 is controlled by the control computer 20. The hardware of the control computer 20 includes a control unit main body 21 having a CPU, ROM, and RAM, a memory 22 including an HDD (may be a built-in HDD), a display panel 23 (output device), a keyboard 24 (input device), and a mouse 25. (Input device) is provided, and the entire device is controlled by firmware or software.

  Control operations and functions related to the present invention will be described separately for each functional block. The control unit 20 includes a power spectrum diagnosis unit 31, a history information storage control unit 32, a history information display control unit 33, and a history information editing control unit 34. And an accessory confirmation unit 35, and the memory 22 includes a history information storage area 41 and a setting information storage area 42.

  First, the power spectrum diagnosis unit 31 and the history information storage control unit 32 will be described. The FTIR 10 loads an initialization program when the apparatus is activated (or at the time of manual initialization operation), and an initialization process including a self-diagnosis function is executed. At this time, the power spectrum diagnostic unit 31 performs power spectrum measurement, performs pass / fail determination based on the measurement result, and controls to display the determination result on the screen.

That is, when power spectrum measurement is started, measurement is performed without a sample in the measurement chamber 13, an interferogram of interference light is obtained, and Fourier transform is performed to obtain measurement data of a power spectrum intensity value. It is done.
And from the obtained the measurement data, three specific wave number used for acceptance judgment ^{(3000cm -1, 2000cm -1, 1000cm} -1) extracts the measured value in. In the setting information storage area 42, standard values of three specific wave numbers (input set values) are stored in advance. The standard values of the three specific wave numbers are compared with the measured actual values, and it is determined whether or not all the actual measured values are equal to or greater than the standard value.

Specifically, for example, by setting a standard value 15.000 for standard value 50.000, wavenumber 1000 cm ^-1 for the standard value 20.000, wavenumber 2000 cm ^-1 for the wave number 3000 cm ^-1 as a standard value Therefore, it is determined whether the measured values at these three points are all equal to or higher than the corresponding standard values.

  The history information storage control unit 32 associates the measurement data of the power spectrum intensity value (actual measurement value) acquired this time with information related to the date and time when the data was measured, and stores it in the history information storage area 41 of the memory 22 as “history information”. Perform accumulation control. If the measurement data of the power spectrum intensity value has been measured in the past and accumulated in the history information storage area 41, the current history information is newly added to the history information accumulated in the past.

Then, the power spectrum diagnostic unit 31 displays the determination result on the display panel 23. At this time, the standard value and the actual measurement value of this time are displayed, and extracted from the history information accumulated in the history information storage area 41 until the previous measurement, or obtained by calculating from these history information. "History reference value" is read and displayed simultaneously with the measurement data (actual measurement value) displayed this time.
As the history reference value, “last measured value” is displayed by default. Note that by changing the setting, instead of this, an “average value” of past measurement data (actually measured values) can be calculated and displayed. It is also possible to extract and display the “highest value” from the first time to the previous time. It is also possible to display the “input value” manually input separately for reference.

FIG. 2 is a diagram illustrating a screen display example in which the determination result is displayed when power spectrum measurement is executed in the initialization process.
In this example, “previous” actual measurement values are displayed side by side below “current” actual measurement values as history reference values. Thereby, the transition of the actual measurement value from the previous time becomes clear together with the determination result of this time. If there is a significant change from the previous actual measurement value, it becomes possible to suspect an optical axis shift or the like.

  In the history reference value in the display example shown in FIG. 2, only the previous actual measurement value is displayed, but a plurality of history reference values may be displayed. For example, the previous actual measurement value and the previous actual measurement value may be displayed as the history reference value, or the previous actual measurement value and the past average value may be displayed as the history reference value.

Next, the history information display control unit 33 and the history information edit control unit 34 will be described.
The history information display control unit 33 performs control to display a list of history information stored in the history information storage area 41 on the screen by sending a display request signal for displaying history information whenever necessary by an input operation using the mouse 25 or the like. Do.
FIG. 3 is a diagram showing a screen display example when a list of history information stored in the history information storage area 41 is displayed by a display request signal.
Measured values of specific wave numbers are listed in chronological order in the order of measurement date. This display makes it easy to grasp changes in the power spectrum over time, and makes it easier to predict when parts replacement and optical axis adjustment are required.

  The displayed list screen is also provided with “delete”, “edit unavailable”, and “first time” fields for each measurement date and time so that a check mark can be entered.

  On the history information list screen described above, the history information edit control unit 34 performs an input operation by checking any of “delete”, “edit unavailable”, and “first time”, thereby performing the history information edit control unit 34. The history information is edited to control the history information, and the processing content is changed in the power spectrum measurement processing from the next time.

  That is, when a check mark is entered in the “delete” column and an input operation is performed, the history information of the corresponding measurement date and time is deleted from the history information storage area 41.

Further, when an input operation is performed with a check mark in the “edit unavailable” column, the measurement date / time data is not erased from the history information storage area 41 but is not used as a display target as a history reference value. It is no longer used as data for calculating the average or maximum value.
By executing the history information editing function as described above, when abnormal measured values are generated due to obvious mistakes, abnormal measured values are not included in the calculation of history reference values such as average values. be able to.

In addition, if an input operation is performed with a check mark (only one place) in the “first time” field, the data is not deleted from the history information storage area 41, but the first measurement when the data of the measurement date and time calculates the history reference value. The history reference value is calculated only from the data measured thereafter. For example, when the optical axis is readjusted, history information before the adjustment time can be excluded by setting “first time”.
On the other hand, once the check marks of “unusable for editing” and “first time” once entered are removed, the history reference value is used again.

  In addition, a comment field is provided at the bottom of the list screen, text data such as characters can be freely input, and implementation details such as parts replacement and maintenance work can be recorded as “remarks”.

  When the initialization process is newly executed after the history information editing control unit 34 performs editing, the history information after the previous “delete”, “edit unavailable”, and “first time” check marks are put. A history reference value is calculated based on the data in the storage area 41.

  Next, the accessory confirmation unit 35 will be described. When a detection signal indicating that the measurement accessory is attached is issued by the accessory sensor 13a of the measurement chamber 13, the accessory confirmation unit 35 detects this signal. In this case, when power spectrum measurement is performed by the power spectrum diagnosis unit 31, the accessory confirmation unit 35 is set to either “delete” or “edit unavailable” via the history information editing control unit 34. Perform processing when a check mark is entered. For example, if the initial setting is set so that "Editing unavailable" is checked, the measurement data when the measurement accessory is attached will not be used for calculation of the history reference value, etc. . When “Delete” is checked, the history information storage area 41 is deleted. Therefore, even when the power spectrum is measured with the measurement accessory attached erroneously, it is possible to calculate the history reference value of only the history information in the normal state where the measurement accessory is not attached.

In the above, an example of the history information display function and editing function according to the present invention has been described. However, the present invention is not limited to this, and various modifications can be made.
For example, in the above-described embodiment, an example in which the spectrophotometer is an FTIR is shown. However, the present invention is not limited to this, and a single-beam visible ultraviolet spectrophotometer and other spectrophotometers can also be applied.
In addition, although the measurement date / time information associated with the measurement data is the date / time, it may include year, minute and second.

  The present invention can be applied to a spectrophotometer such as FTIR.

10 FTIR (spectrophotometer)
DESCRIPTION OF SYMBOLS 11 Light source 12 Interferometer 13 Measurement chamber 13a Accessory sensor 15 Detector 20 Control part 31 Power spectrum diagnostic part 32 History information storage control part 33 History information display control part 34 History information edit control part 35 Accessory confirmation part 41 History information storage Area 42 Setting information storage area

Claims (3)

A power spectrum that compares the measured value of the power spectrum intensity obtained from the detection signal measured when the light emitted from the light source is incident on the detector without passing through the sample, and a preset standard value of the power spectrum intensity the strength measurement tests, a spectrophotometer equipped with a power spectrum diagnostic unit to run when initializing the at least spectrophotometer,
A history information storage control unit for storing the measured value of the power spectrum intensity as history information together with the date and time information on which the detection was performed;
A history information display control unit that displays the history information when receiving a display request signal ,
The history information display control unit, when a new power spectrum intensity measurement test is executed, together with the newly detected actual value of the power spectrum intensity, the previous actual value, or the average value until the previous time, or the history information Displays one of the historical reference values of the reference values obtained by performing arithmetic processing using
Further, the history information stored by the history information storage control unit can execute an editing function for deleting a part of the history information, and the calculation process without deleting the part of the history information. A spectrophotometer comprising a history information editing control unit capable of executing an editing function for selecting whether to use or not . The spectrophotometer includes an accessory sensor that detects whether or not a measurement accessory is attached, and an accessory confirmation unit that checks the presence or absence of a measurement accessory based on a signal from the accessory sensor, and the history information The edit control unit deletes the power spectrum intensity measurement test when the accessory confirmation unit confirms the mounting of the measurement accessory so that it is not included in the history information, or uses it in the editing function. The spectrophotometer according to claim 1 , wherein the editing function is executed by removing the spectrophotometer. The spectrophotometer according to claim 1 or 2, wherein the spectrophotometer is FTIR.

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