JP3379340B2 - Sample filling device in spectrometer - Google Patents

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a spectrometer for analyzing components such as grains and quality using a spectrometer, and more particularly, to sample filling in the spectrometer. Related to the device. 2. Description of the Related Art Conventionally, a sample filling apparatus for analyzing components such as grains and quality using such a spectroscopic analyzer has been known.
After the sample is packed in the sample container, the sample is set at the measurement position of the spectrometer and the measurement is performed.However, this requires the operator to pack the sample into the sample container, which is troublesome. It took. In addition, since there is an individual difference in how to pack the sample depending on the measurer, an error may occur in the measurement result. In order to solve the above-mentioned problems, as shown in FIG. 5, in order to reduce a measurement error due to a non-uniform density of a sample in a sample container 32, light emitted from a light source 31 is reduced. Focusing on 32 samples, moving the optical axis vertically in multiple steps intermittently with respect to the sample, detecting optical measurements at each stationary step during the intermittent movement, A method in which the average value of a plurality of measured values is adopted as a measured value for a sample (Japanese Patent Application Laid-Open No. 8-43299) has been proposed. Since the measurement is performed, a large error occurs in a plurality of detected measurement values. Thus this device, and detects a measurement result by averaging a plurality of measurements large errors were saying Enaka' from those capable of detecting a good measurement results with high accuracy. In order to automate the filling of the sample container with the sample, a funnel-shaped hopper is provided above the sample container formed of a transparent member, and a slide shutter is provided below the hopper. There is a sample filling device that supplies the sample to the sample container. However, when the shutter is closed to stop the supply of the sample to the sample container, the shutter is sandwiched between the sample and the shutter. There was a problem that it could not be completely closed. [0005] From the above, according to the present invention, by using a simple structure, the supply of the sample into the sample case is automated, the operation is simplified, and the operation is simplified. It is an object of the present invention to provide a sample filling apparatus in a spectroscopic analyzer which can minimize a measurement error caused by uneven density in the past by making the density of the sample in the sample case uniform. I do. [0006] In order to solve the above problems, the present invention provides a sample case which is connected to a hopper into which a sample is charged and which is filled with a sample falling from the hopper. In a spectroscopic analyzer that measures reflected light or transmitted light by irradiating light of a required wavelength to a case, in the hopper, a sample input port provided with a cut gate shutter at the bottom is provided, and at the bottom of the sample case. the rotary valve for forcibly discharging the sample in the sample case by a certain amount is provided, prior to measuring the lowest by the rotary valve
Technical measures were taken to discharge the layer sample . When the sample has been put into the hopper, the cut gate shutter at the sample inlet is opened for a certain period of time to fill the sample into the sample case. At this time, the shutter, because of the use of cut-gate shutter for opening and closing by a driving device, not abruptly stop the shutter by biting of the sample.
Further, the cut gate shutter shields the inside of the sample case from light so as to prevent unnecessary light from being incident on the measurement unit, thereby preventing a measurement error from occurring. By the way, as a result of the experiment, the lower part and the upper part of the sample case have a high density at the lowermost part due to the difference in the pile height of the sample, and the other upper parts have a relatively low density. It turned out that the phenomenon of being stable on average occurred. Although in order to measure accurately, it is necessary to measure at a plurality of locations, if the density is different at the upper and lower layer as described above, it will cause an error occurs by itself. [0008] A sample is put into the sample case, and after a predetermined time, the cut gate shutter is closed, and the rotary valve provided at the lower portion of the sample case starts rotating to forcibly discharge the sample in the lowermost layer of the sample case. As described above, by discharging the sample of the relatively high-density portion in the lowermost layer first, the relatively low-density and stable layer descends downward, so that the density of the sample in the sample case is reduced. It can be uniform. Then, when the rotary valve stops, the light emitted from the light source is irradiated on the irradiation window formed of the transparent member, and the light transmitted between the samples located in the irradiation window is received by the light receiving device, and the measured value is measured. To detect. When the first measurement is completed, the rotary valve is rotated by an angle (for example, 90 degrees), and the sample stored in the rotary valve is discharged. At this time, since the rotary valve has a plurality of blades radially attached around the rotation axis of the valve to form an empty space for accommodating the sample between the blades, a certain amount of the sample is stored in the empty room. Always filled. Therefore, the rotary valve can discharge a certain amount of sample at any time. As a result of such a quantitative discharge operation, the sample located at the measurement site falls, and the sample in the upper layer of the sample case gradually falls. When the work of discharging such a fixed amount is completed, the measurement of the sample is performed in the same manner as the previous time. After these operations are repeated several times, the obtained measurement values are averaged to detect the measurement result, and all the samples in the sample case are discharged to complete the measurement operation. In FIG. 1, reference numeral 1 denotes a sample placed in a hopper 2, a sample is dropped and filled into a sample case 7 connected to the hopper 2, and the sample case 7 having a required wavelength is filled. 1 shows the entirety of a spectroscopic analyzer that irradiates light and measures transmitted light or reflected light that has transmitted through a sample, and has a configuration in which a supply unit 41 is provided above the spectroscopic analyzer 1 and the supply unit 41 is provided. Is provided with a measuring section 42, a light receiving section 43 is provided on one side and a light source section 44 is provided on the other side of the measuring section 42, and a discharge section 45 is provided below the measuring section 42. Further, details of the above configuration will be described. The supply unit 41 shown in FIG. 2 and FIG.
It comprises a sample inlet 3, a cut gate shutter 5, and a soundproof material 6. The hopper 2 has a funnel shape, and is provided with a sample inlet 3 into which a sample to be measured is inserted. A drive device, for example, a cut gate shutter 5 that is opened and closed by a solenoid 4 is provided below the sample inlet 3, and a soundproof material 6 for preventing metal noise generated by an impact when the cut gate shutter 5 is opened and closed. Are provided on both outer slopes of the sample inlet 3. The upper ends of the hopper 2 and the sample inlet 3 are joined to each other . The measuring section 42 shown in FIGS. 1 and 4 comprises a sample case 7, an irradiation window 8 and a sensor 9. The top of the sample case 7 in communication with the lower portion of the hopper 2, the shape of the sample case 7 are circular, elliptical, cross-section of rectangular or square. In the center of the side surface of the sample case 7, irradiation windows 8A and 8B made of a transparent member, for example, glass are fitted so as to face each other. Further, sensors 9 for detecting the degree of clogging of the sample are provided at the upper and lower portions of the side surface of the sample case 7, respectively. Similarly, the light receiving section 4 shown in FIGS.
Reference numeral 3 denotes a light receiving device for performing measurement by receiving light transmitted from the light source 48 through the sample through one irradiation window 8A and passing through the light receiving unit 43 through the other irradiation window 8B. 21
It is composed of The light receiving device 21 is provided outside the sample case 7 so as to surround the irradiation window 8B fitted to the central side surface of the sample case 7. The light source section 44 shown in FIG.
(See FIG. 4), and is constituted by a filter section 47 and a light source body 48. The cylinder portion 46 is formed by the cylinder 10 and the diffusion lens 20. The cylindrical body 10 has an irradiation window 8A.
Is connected to the sample case 7 so as to surround the irradiation window 8.
A light path to A is formed, and the light path is provided so that light is perpendicularly incident on the irradiation window 8A. Also,
The diffusion lens 20 is provided on the optical path to irradiate the entirety of the irradiation window 8A with the converged light having a required wavelength that has passed through the filter. The filter section 47 includes disks 16A and 16B having a plurality of filters on the circumference thereof,
A and B are formed by motors 17A and 17B for driving A and B, respectively. The disk 16A has a plurality of NDs in the circumferential direction of the disk.
Similarly, a plurality of bandpass filters 15 are provided on the filter 14 and the disk 16B, respectively. The N
The D filter 14 is used for calibrating the optical system and the light detection circuit, and acts so that strong light does not directly enter the detector. The band pass filter 15 transmits only a required wavelength. The shafts 18A and 18B of the motors 17A and B for driving the disks 16A and 16B are directly connected to the centers of the disks 16A and 16B, respectively.
Is provided, and by controlling the rotation of the motors 17A, B, a plurality of filters provided on the disks 16A, 16B are switched. Then, the two types of filters are used as the condenser lens 1
The filter section 47 is arranged so as to be located on the optical path of the light converged in 3 and between the cylindrical body section 46 and the light source body 48. The light source 48 includes a halogen lamp 11,
The cooling fin 12 and the condenser lens 13 are formed. A halogen lamp 11 as a light source is provided toward the sample case 7, and around the halogen lamp 11,
A cooling fin 12 for diffusing heat generated from the halogen lamp 11 is provided, and a condenser lens 13 for condensing light emitted from the halogen lamp 11 is provided in an optical path between the halogen lamp 11 and the disk 16. Provided. The discharge section 45 shown in FIGS. 1 and 4 comprises a rotary valve 25 and a grain collecting box 26. The rotary valve 25 has a plurality of cavities 24 formed by a plurality of blades 23 radially mounted around a rotation shaft 22 of a driving device (not shown). Further, the rotary valve 25 is rotatably provided below the sample case 7, and a grain collecting box 26 for storing the sample discharged from the rotary valve 25 is provided below the rotary valve 25. In this embodiment, a tabletop spectroscopic analyzer is shown, but it can be used not only on a table but also as a tester in a post-process of the analyzer for measuring the particle size of a sample. . Hereinafter, a specific operation of the above configuration will be described. When a sample is inserted into the sample inlet 3, the cut gate shutter 5 is opened for a certain period of time after the end of the injection, and the sample in the hopper 2 is filled in the sample case 7 connected to the hopper 2. At this time, the cut gate shutter 5, to hit the soundproofing material 6 immediately before as possible fully open, cut gate
An unpleasant metal sound due to the impact of the shutter 5 does not occur. [0020] finishes put the sample in the sample case 7
After a certain period of time, the cut gate shutter 5 closes, and the rotary valve 25 rotates, for example, about 135 degrees (an angle of three empty chambers 24 formed between the blades 23) . Due to the rotation of the rotary valve 25, a relatively high-density sample in the lowermost layer in the sample case 7, which has been generated due to a difference in sample deposition height, is first discharged into the grain collection box 26, and The density difference in the sample case 7 between the upper layer and the lower layer in the sample case 7 is eliminated to make the density in the sample case 7 substantially uniform (see FIG. 4). Also,
When two sensors 9 provided on the upper and lower sides of the sample case 7 detect whether or not there is enough sample in the sample case 7 to perform measurement, and when any one of them is not detected. Displays a message (eg, not shown) that warns the user to add a sample as an error message.
To be displayed. If no error message is displayed, it means that the amount of the sample to be measured in the sample case 7 is sufficient, and the measurement operation is started. The diffused light emitted from the halogen lamp 11 is converged by the condenser lens 13 into light having a certain width, and the converged light passes through the ND filter 14 and the band-pass filter 15 so that it is required. Only light of the wavelength. The focused light of the required wavelength is diffused by the diffusion lens 20 so as to irradiate the entire irradiation window 8A. The light that has entered the sample case 7 from the irradiation window 8A passes between the samples, and the transmitted light passes through the irradiation window 8B and enters the light receiving device 21 for measurement. At this time, since the upper ends of the sample inlet 3 and the hopper 2 are in contact with each other, light other than the light emitted from the halogen lamp 11 enters the light receiving device 21. Never. When the first measurement is completed, the rotary valve 25 is rotated to remove a small amount of the sample in the grain collection box in order to replace the sample near the irradiation window 8 where the measurement has been performed with as many unmeasured samples as possible. Discharge into 26. At this time, by rotating the rotary valve 25 by 90 degrees, many samples located near the irradiation window 8 fall to the lower part of the sample case 7.
The unmeasured sample in the upper layer of the sample case 7 sequentially falls into the portion. At this time, the rotary valve 25 has a plurality of blades 23 radially mounted around the rotation shaft 22 to form a space 24 for accommodating a sample between the blades 23. A certain amount of sample is always filled. Therefore, the rotary valve 25 can discharge a fixed amount of sample at any time.
Then, when the discharge of such a fixed amount is completed, the measurement of the sample is performed in the same manner as the previous time. After the measurement of the sample is performed, for example, three times, the measured values of the three times are averaged to detect the measurement result, and all the samples in the sample case 7 are discharged to the grain collection box 26 to obtain one sample. Measurement operation is completed. According to the present invention, the sample inlet is provided inside the hopper with a cut gate shutter at the lower part, so that the operation of supplying the sample to the sample case is automated and the operation is simplified.
In addition, a rotary valve is provided below the sample case to forcibly discharge the sample in the sample case by a fixed amount, and the lowermost layer of the sample case having a relatively high density is discharged by the rotary valve. The density of the sample, which is different between the upper layer and the lower layer, can be made substantially uniform, and the measurement error which has been caused by the non-uniform density can be reduced as much as possible, and a highly accurate measurement result can be obtained. By using the cut gate shutter provided at the lower part of the sample inlet, the sample can be supplied to the sample case many times in the same manner, so that the filling which has been conventionally caused by the measurer is performed. There is no unevenness, and no accident of stopping the shutter due to biting of the sample. Further, since the cut gate shutter increases the light shielding property in the sample case, a measurement error caused by external light entering the sample case becomes smaller. In addition, by using a rotary valve having an empty space formed by a plurality of blades mounted radially about a rotation axis, a fixed amount of sample can be easily and reliably discharged. it can.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a sectional view showing an embodiment of the present invention. FIG. 2 is an enlarged sectional view showing an open / closed state of a cut gate shutter in FIG. FIG. 3 is an enlarged view of a cut gate shutter viewed from a direction of an arrow in FIG. 2; FIG. 4 is an enlarged sectional view showing a state where a sample is being discharged from a sample case. FIG. 5 is a sectional view showing a conventional example. [Description of Signs] 1 Spectroscopic analyzer 2 Hopper 3 Sample inlet 4 Solenoid 5 Cut gate shutter 6 Soundproof material 7 Sample case 8 Irradiation window 8A Irradiation window 8B Irradiation window 9 Sensor 10 Tube 11 Halogen lamp 12 Cooling fin 13 Gather Optical lens 14 ND filter 15 Bandpass filter 16A Disk 16B Disk 17A Motor 17B Motor 18A Axis 18B Axis 19A Encoder 19B Encoder 20 Diffusion lens 21 Light receiving device 22 Rotating shaft 23 Blade 24 Vacancy 25 Rotary valve 26 Grain collection box 31 Light source 32 Sample container 41 Supply unit 42 Measurement unit 43 Light receiving unit 44 Light source unit 45 Discharge unit 46 Cylindrical unit 47 Filter unit 48 Light source

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-3-269347 (JP, A) JP-A-58-77637 (JP, A) JP-A-6-207856 (JP, A) JP-A-7-207 140134 (JP, A) JP-A-1-150835 (JP, A) JP-A-8-43299 (JP, A) JP-A-10-30984 (JP, A) (58) Fields investigated (Int. Cl. ^7, DB name) G01N 1/00 101 G01N 21/01 G01N 21/27 JICST file (JOIS)

Claims (1)

(57) [Claim 1] A sample case is provided which is connected to a hopper into which a sample is put and which is filled with a sample falling from the hopper, and the sample case is irradiated with light of a required wavelength. In a spectroscopic analyzer for measuring reflected light or transmitted light, a sample input port provided with a cut gate shutter at a lower portion is provided in the hopper, and a certain amount of the sample in the sample case is provided at a lower portion of the sample case. A rotary valve that forcibly discharges each is provided .
A sample filling device in a spectroscopic analyzer, wherein a sample in a layer portion is discharged .