CN109632854B - Massive uranium ore multi-element online X fluorescence analyzer with double detection structures - Google Patents
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Abstract
本发明涉及一种双探测结构的块状铀矿多元素在线X荧光分析仪,由激发光源、双探测分析装置、传输带、辅助设备组成,其中激发光源包括高功率X光管、设置于X光管出口的准直器、X光管高压;激发光源发出的X射线垂直照射在传送带上的块状铀矿样品,激发块状铀矿样品中不同位置的多元素特征X荧光信息后,被不同探测结构的双探测装置接收。通过双探测结构的耦合模型,能够克服块状铀矿表面凹凸不平带来的几何效应对在线X荧光分析仪分析结果准确度的影响,提高在线X荧光分析仪分析准确度,操作简单,测量快速,精度高,安全环保。
The invention relates to a bulk uranium ore multi-element online X-fluorescence analyzer with double detection structure, which is composed of an excitation light source, a dual detection and analysis device, a transmission belt and auxiliary equipment. The collimator at the outlet of the light tube and the high voltage of the X-ray tube; the X-rays emitted by the excitation light source vertically irradiate the bulk uranium ore sample on the conveyor belt, and after exciting the multi-element characteristic X-fluorescence information at different positions in the bulk uranium ore sample, the Dual detection devices with different detection structures receive. Through the coupling model of the dual detection structure, the influence of the geometric effect caused by the uneven surface of the massive uranium ore on the accuracy of the online X-ray fluorescence analyzer can be overcome, and the analysis accuracy of the online X-ray fluorescence analyzer can be improved. The operation is simple and the measurement is fast. , high precision, safety and environmental protection.
Description
技术领域:Technical field:
本发明涉及一种双探测结构的块状铀矿多元素在线X荧光分析仪,尤其是分析块状样品中多元素含量的在线X荧光分析仪,其属于铀矿元素快速分析领域。The invention relates to a bulk uranium ore multi-element online X-fluorescence analyzer with double detection structure, in particular to an online X-fluorescence analyzer for analyzing the multi-element content in a bulk sample, which belongs to the field of rapid analysis of uranium ore elements.
背景技术:Background technique:
铀矿是我国的战略资源,铀矿品味的快速在线测量尤其重要。但目前大都是基于化学分析方法,一般都需要将样品在高温下燃烧,再用化学试剂与其反应从而计算出铀矿含量。这种基于化学分析方法,由于需要在严格制样过程,所以测量时间较长,由于需要用化学试剂,所以会对环境造成严重污染,对使用人员的身体健康造成损害。Uranium ore is a strategic resource in my country, and rapid online measurement of uranium ore grade is particularly important. However, most of them are based on chemical analysis methods. Generally, the samples need to be burned at high temperature, and then chemical reagents are used to react with them to calculate the uranium ore content. This method based on chemical analysis requires a long measurement time due to the strict sample preparation process. Due to the need to use chemical reagents, it will cause serious pollution to the environment and damage to the health of users.
在线X射线荧光 (X-ray Fluorescence, XRF) 分析技术因其具有实时在线、方便快速、无损测量等优点在实现铀矿实时在线测量方面具有广阔的应用前景。实验室XRF分析中,通常通过不同的制样方法(如压片、熔融、消解等),消除样品本身带来的干扰,但在线XRF分析技术是对现场未知样品的直接测量,没有制样过程,因此在线XRF分析技术准确度的干扰因素主要来源于样品本身如含形状大小不一表面凹凸不平(几何效应)、样品成分复杂等。同时,为了提高块状物料XRF在线测量的准确度,必须对以上干扰因素进行校正。实验室分析中,该影响可以通过特定的制样方法如熔融、消解等来消除,但在线XRF分析,没有制样过程,因此针对块状物料,要提高在线XRF分析技术的测量准确度,解决几何效应刻不容缓。On-line X-ray Fluorescence (XRF) analysis technology has broad application prospects in real-time on-line measurement of uranium ore due to its advantages of real-time on-line, convenient, rapid, and non-destructive measurement. In laboratory XRF analysis, different sample preparation methods (such as tableting, melting, digestion, etc.) are usually used to eliminate the interference caused by the sample itself, but online XRF analysis technology is a direct measurement of unknown samples on site, and there is no sample preparation process. Therefore, the interference factors of the accuracy of the online XRF analysis technology mainly come from the sample itself, such as the uneven surface (geometric effect) of different shapes and sizes, and the complex composition of the sample. At the same time, in order to improve the accuracy of XRF online measurement of bulk materials, the above interference factors must be corrected. In laboratory analysis, this effect can be eliminated by specific sample preparation methods such as melting and digestion, but online XRF analysis does not have a sample preparation process. Therefore, for bulk materials, it is necessary to improve the measurement accuracy of online XRF analysis technology to solve the problem. The geometric effect is urgent.
因此,确有必要对现有技术进行改进以解决现有技术之不足。Therefore, it is indeed necessary to improve the existing technology to solve the shortcomings of the existing technology.
发明内容:Invention content:
本发明提供一种无化学污染、无放射性污染、测量时间短、精度高、结构简单、安全可靠的双探测结构的块状铀矿多元素在线X荧光分析仪。The invention provides a massive uranium ore multi-element online X-fluorescence analyzer with double detection structure without chemical pollution, without radioactive pollution, short measurement time, high precision, simple structure, safety and reliability.
本发明采用如下技术方案:一种双探测结构的块状铀矿多元素在线X荧光分析仪,该分析仪包括激发光源、双探测分析装置、传输带、辅助设备,所述激发光源包括X光管、X光管高压,辅助设备包括船型雪橇刮板和激光测距仪,船型雪橇刮板固定设在传输带的上方,激光测距仪设在船型雪橇刮板的一侧,X光管和X光管高压设在在船型雪橇刮板上,所述双探测分析装置包括两个探测系统:反射式探测系统和透射式探测系统,反射式探测系统包括硅漂移探测器、探测器高压、与硅漂移探测器连接的电荷灵敏前置放大器、与电荷灵敏前置放大器连接的脉冲成型放大器及与脉冲成型放大器连接的数字化多道谱仪,硅漂移探测器在X光管的一侧;透射式探测系统包含碲化镉探测器、探测器高压、与碲化镉探测器连接的电荷灵敏前置放大器、与电荷灵敏前置放大器连接的脉冲成型放大器及与脉冲成型放大器连接的数字化多道谱仪,碲化镉探测器在传输带的下方;双探测系统收集的能谱信息都转化为用于分析的能谱并由计算机进行数据处理控制;所述传输带用于块状铀矿样品在线输送;船型雪橇刮板采用物理重力原理压平较大的块状铀矿样品,激光测距仪进行辅助判断块状铀矿几何变化,为不同探测系统提供判断依据。The present invention adopts the following technical scheme: a bulk uranium ore multi-element online X-fluorescence analyzer with dual detection structure, the analyzer includes an excitation light source, a dual detection analysis device, a transmission belt, and auxiliary equipment, and the excitation light source includes X-rays Tube and X-ray tube are high pressure, auxiliary equipment includes boat-shaped sled scraper and laser range finder, the boat-shaped sled scraper is fixed above the conveyor belt, the laser range finder is set on one side of the boat-shaped sled scraper, X-ray tube and The high-voltage X-ray tube is set on the scraper of the boat-shaped sled. The dual detection and analysis device includes two detection systems: a reflection detection system and a transmission detection system. The reflection detection system includes a silicon drift detector, a detector high voltage, and a A charge-sensitive preamplifier connected to the silicon drift detector, a pulse shaping amplifier connected to the charge-sensitive preamplifier, and a digital multi-channel spectrometer connected to the pulse shaping amplifier, the silicon drift detector is on one side of the X-ray tube; transmission type The detection system includes a cadmium telluride detector, a detector high voltage, a charge sensitive preamplifier connected with the cadmium telluride detector, a pulse shaping amplifier connected with the charge sensitive preamplifier, and a digital multi-channel spectrometer connected with the pulse shaping amplifier , the cadmium telluride detector is below the transmission belt; the energy spectrum information collected by the dual detection system is converted into the energy spectrum for analysis and controlled by the computer for data processing; the transmission belt is used for online transportation of bulk uranium ore samples The ship-shaped sled scraper uses the principle of physical gravity to flatten the larger bulk uranium ore samples, and the laser range finder assists in judging the geometric changes of the bulk uranium ore, providing a basis for different detection systems.
反射式探测系统和透射式探测系统,采用激光测距仪进行辅助判断块状铀矿几何变化,当块状铀矿几何变化在20mm以内时采用反射式测量,当X光管发出的X射线照射在块状铀矿样品上,激发铀矿的特征X荧光信息,荧光信息被硅漂移探测器接收,经电荷灵敏前置放大器、脉冲成型放大器成形放大后由数字化多道谱仪转化为用于分析的能谱;当块状铀矿几何变化范围在20mm--100mm时,透射式起到作用,当X光管发出的X射线照射在块状铀矿样品上,激发铀矿的特征X荧光信息,荧光信息被碲化镉探测器接收,经电荷灵敏前置放大器、脉冲成型放大器成形放大后由数字化多道谱仪转化为用于分析的能谱;计算机通过分析激光测距仪的距离信息,利用不同探测器对X荧光的探测响应及不同能量的特征X荧光信息的穿透能力建立双探测结构的耦合模型,克服块状铀矿表面凹凸不平带来的几何效应效应对样品中多元素的特征X荧光强度的影响,提高在线X荧光分析仪分析准确度。The reflective detection system and the transmission detection system use a laser rangefinder to assist in judging the geometric change of the massive uranium ore. When the geometric change of the massive uranium ore is within 20mm, the reflective measurement is used. On the bulk uranium ore sample, the characteristic X fluorescence information of the uranium ore is excited, and the fluorescence information is received by the silicon drift detector. When the geometric variation range of the massive uranium ore is 20mm--100mm, the transmission type plays a role. When the X-ray emitted by the X-ray tube is irradiated on the massive uranium ore sample, the characteristic X fluorescence information of the uranium ore is excited. , the fluorescence information is received by the cadmium telluride detector, and after being shaped and amplified by the charge-sensitive preamplifier and the pulse shaping amplifier, it is converted into the energy spectrum for analysis by the digital multi-channel spectrometer; the computer analyzes the distance information of the laser rangefinder, Using the detection response of different detectors to X-fluorescence and the penetrating ability of characteristic X-fluorescence information of different energies, a coupled model of dual detection structure is established to overcome the geometric effect caused by the uneven surface of the massive uranium ore, which has a negative impact on the multi-element in the sample. The influence of characteristic X fluorescence intensity improves the analysis accuracy of online X fluorescence analyzer.
所述硅漂移探测器的铍窗为0.4毫米,探测范围为1-30keV。The beryllium window of the silicon drift detector is 0.4 mm, and the detection range is 1-30 keV.
所述碲化镉探测器的铍窗为0.5毫米,探测范围为20-100keV。The beryllium window of the cadmium telluride detector is 0.5 mm, and the detection range is 20-100 keV.
激光测距仪量程为0—100mm,精度为0.07mm,固定在船型雪橇刮板上进行辅助判断块状铀矿几何变化,为不同探测系统提供判断依据。The laser range finder has a range of 0-100mm and an accuracy of 0.07mm. It is fixed on the ship-shaped sled scraper to assist in judging the geometric changes of massive uranium ore, and provides a basis for different detection systems.
所述的X光管高压为80000伏。The high voltage of the X-ray tube is 80,000 volts.
所述硅漂移探测器与块状铀矿样品之间距离为6毫米,夹角为90度。The distance between the silicon drift detector and the bulk uranium ore sample is 6 mm, and the included angle is 90 degrees.
所述碲化镉探测器与块状铀矿样品之间距离为5毫米,夹角为90度。The distance between the cadmium telluride detector and the bulk uranium ore sample is 5 mm, and the included angle is 90 degrees.
所述船型雪橇刮板采用厚度5mm的钢板,重量大于或等于100kg。The boat-shaped ski scraper adopts a steel plate with a thickness of 5mm, and the weight is greater than or equal to 100kg.
所述传输带厚度为5mm。The thickness of the conveyor belt is 5mm.
本发明具有如下有益效果:与现有X荧光设备相比,采用高功率X光管作为激发光源,不产生化学污染和放射性污染;与现有X荧光设备相比,采用双探测系统克服块状铀矿表面凹凸不平带来的几何效应效应对样品中多元素的特征X荧光强度的影响,提高在线X荧光分析仪分析准确度;由于采用现今较为先进的硅漂移和碲化镉探测器以及多道分析器,所以精度高,测量范围更广,人为误差小,操作者劳动强度低;采用激光测距仪实时监测样品表面变化程度,提高在线X荧光分析仪分析准确度;本发明不需要制样过程,直接在线测量,速度快、结果准确。The invention has the following beneficial effects: compared with the existing X-ray fluorescence equipment, a high-power X-ray tube is used as the excitation light source, and no chemical pollution and radioactive pollution are produced; The geometric effect caused by the uneven surface of uranium ore affects the characteristic X-fluorescence intensity of multiple elements in the sample, and improves the analysis accuracy of the online X-fluorescence analyzer; due to the use of the more advanced silicon drift and cadmium telluride detectors and many It uses a laser range finder to monitor the change degree of the sample surface in real time, so as to improve the analysis accuracy of the online X-ray fluorescence analyzer; the present invention does not need to manufacture The sample process is directly measured online, with fast speed and accurate results.
附图说明:Description of drawings:
图l 为本发明工作原理图。Fig. 1 is a working principle diagram of the present invention.
图2 为本发明硅漂移探测系统能谱图。FIG. 2 is an energy spectrum diagram of the silicon drift detection system of the present invention.
图3 为本发明碲化镉探测器系统能谱图。FIG. 3 is an energy spectrum diagram of the cadmium telluride detector system of the present invention.
其中:in:
1- X光管;2-光管高压;3-硅漂移探测器;4-探测器高压;5-电荷灵敏前置放大器;6-脉冲成型放大器;7-碲化镉探测器;8-探测器高压;9-电荷灵敏前置放大器;10-脉冲成型放大器;11-数字化多道谱仪;12-激光测距仪;13-传输带;14-铀矿样品;15-船型雪橇刮板;16-计算机。1- X-ray tube; 2- Light tube high voltage; 3- Silicon drift detector; 4- Detector high voltage; 5- Charge sensitive preamplifier; 6- Pulse shaping amplifier; 7- Cadmium telluride detector; 8- Detection 9-charge sensitive preamplifier; 10-pulse shaping amplifier; 11-digital multi-channel spectrometer; 12-laser rangefinder; 13-transmission belt; 14-uranium ore sample; 15-boat sled scraper; 16 - Computer.
具体实施方式:Detailed ways:
请参照图1至图3所示,一种双探测结构的块状铀矿多元素在线X荧光分析仪,其包括激发光源、双探测分析装置、传输带、辅助设备,所述激发光源包括X光管、X光管高压;所述双探测分析装置包括两个探测系统(反射式和透射式),反射式探测系统设置于X光管右边的硅漂移探测器、探测器高压、与硅漂移探测器连接的电荷灵敏前置放大器、与电荷灵敏前置放大器连接的脉冲成型放大器及与脉冲成型放大器连接的数字化多道谱仪,透射式探测系统包含传输带下方的碲化镉探测器、探测器高压、与碲化镉探测器连接的电荷灵敏前置放大器、与电荷灵敏前置放大器连接的脉冲成型放大器及与脉冲成型放大器连接的数字化多道谱仪,双探测系统收集的能谱信息都转化为用于分析的能谱并由计算机进行数据处理控制;所述传输带主要用于块状铀矿样品在线输送;辅助设备包括船型雪橇刮板和激光测距仪,船型雪橇刮板用于固定在线X荧光分析仪并采用物理重力原理压平较大块状铀矿样品,激光测距仪进行辅助判断块状铀矿几何变化,为不同探测系统提供判断依据。Please refer to FIG. 1 to FIG. 3 , a bulk uranium ore multi-element online X-ray fluorescence analyzer with dual detection structure, which includes an excitation light source, a dual detection analysis device, a transmission belt, and auxiliary equipment, and the excitation light source includes X High voltage of light tube and X-ray tube; the double detection and analysis device includes two detection systems (reflection type and transmission type). A charge-sensitive pre-amplifier connected to the detector, a pulse-shaping amplifier connected to the charge-sensitive pre-amplifier, and a digital multi-channel spectrometer connected to the pulse-shaping amplifier, the transmission detection system includes a cadmium telluride detector below the transmission belt, a detection high voltage, charge sensitive preamplifier connected to the cadmium telluride detector, pulse shaping amplifier connected to the charge sensitive preamplifier, and digital multi-channel spectrometer connected to the pulse shaping amplifier, the energy spectrum information collected by the dual detection system is all It is converted into energy spectrum for analysis and controlled by computer for data processing; the conveyor belt is mainly used for online transportation of bulk uranium ore samples; auxiliary equipment includes ship-shaped sled scraper and laser range finder, and the ship-shaped sled scraper is used for The online X-ray fluorescence analyzer is fixed and the larger bulk uranium ore samples are flattened by the principle of physical gravity, and the laser rangefinder is used to assist in judging the geometric changes of the bulk uranium ore, providing a basis for different detection systems.
本发明中提出双探测结构(反射式和透射式),采用激光测距仪进行辅助判断块状铀矿几何变化,当块状铀矿几何变化在20mm以内时采用反射式测量,当X光管发出的X射线照射在块状铀矿样品上,激发铀矿的特征X荧光信息,荧光信息被硅漂移探测器接收,经电荷灵敏前置放大器、脉冲成型放大器成形放大后由数字化多道谱仪转化为用于分析的能谱;当块状铀矿几何变化范围在20mm--100mm时,透射式起到主要作用,当X光管发出的X射线照射在块状铀矿样品上,激发铀矿的特征X荧光信息,荧光信息被碲化镉探测器接收,经电荷灵敏前置放大器、脉冲成型放大器成形放大后由数字化多道谱仪转化为用于分析的能谱;计算机通过分析激光测距仪的距离信息,利用不同探测器对X荧光的探测响应及不同能量的特征X荧光信息的穿透能力建立双探测结构的耦合模型,克服块状铀矿表面凹凸不平带来的几何效应效应对样品中多元素的特征X荧光强度的影响,提高在线X荧光分析仪分析准确度。In the present invention, a dual detection structure (reflection type and transmission type) is proposed, and a laser range finder is used to assist in judging the geometric change of the massive uranium ore. The emitted X-rays are irradiated on the bulk uranium ore sample to excite the characteristic X-fluorescence information of the uranium ore. The fluorescence information is received by the silicon drift detector. It is converted into an energy spectrum for analysis; when the geometric variation range of the massive uranium ore is 20mm--100mm, the transmission type plays a major role. The characteristic X fluorescence information of the ore, the fluorescence information is received by the cadmium telluride detector, shaped and amplified by the charge-sensitive preamplifier and the pulse shaping amplifier, and then converted into the energy spectrum for analysis by the digital multi-channel spectrometer; The distance information from the instrument, the detection response of different detectors to X-fluorescence and the penetrating ability of characteristic X-fluorescence information of different energies are used to establish a coupling model of dual detection structure to overcome the geometric effect caused by the uneven surface of massive uranium ore The influence on the characteristic X fluorescence intensity of multiple elements in the sample improves the analysis accuracy of the online X fluorescence analyzer.
本发明双探测结构的块状铀矿多元素在线X荧光分析仪的工作原理为:本发明中提出双探测结构(反射式和透射式),采用激光测距仪进行辅助判断块状铀矿几何变化,当块状铀矿几何变化在20mm以内时采用反射式测量,当X光管发出的X射线照射在块状铀矿样品上,激发铀矿的特征X荧光信息,荧光信息被硅漂移探测器接收,经电荷灵敏前置放大器、脉冲成型放大器成形放大后由数字化多道谱仪转化为用于分析的能谱;当块状铀矿几何变化范围在20mm--100mm时,透射式起到主要作用,当X光管发出的X射线照射在块状铀矿样品上,激发铀矿的特征X荧光信息,荧光信息被碲化镉探测器接收,经电荷灵敏前置放大器、脉冲成型放大器成形放大后由数字化多道谱仪转化为用于分析的能谱;计算机通过分析激光测距仪的距离信息,利用不同探测器对X荧光的探测响应及不同能量的特征X荧光信息的穿透能力建立双探测结构的耦合模型,克服块状铀矿表面凹凸不平带来的几何效应效应对样品中多元素的特征X荧光强度的影响,提高在线X荧光分析仪分析准确度。The working principle of the massive uranium ore multi-element on-line X-fluorescence analyzer with dual detection structure of the present invention is as follows: a dual detection structure (reflection type and transmission type) is proposed in the present invention, and a laser range finder is used to assist in judging the geometry of the massive uranium ore. When the geometric change of the massive uranium ore is within 20mm, the reflection measurement is adopted. When the X-ray emitted by the X-ray tube is irradiated on the massive uranium ore sample, the characteristic X-fluorescence information of the uranium ore is excited, and the fluorescence information is detected by the silicon drift. It is received by the digital multi-channel spectrometer after being shaped and amplified by the charge-sensitive preamplifier and the pulse shaping amplifier, and converted into an energy spectrum for analysis; when the geometric variation range of the massive uranium ore is 20mm--100mm, the transmission type plays the role of The main function is that when the X-ray emitted by the X-ray tube is irradiated on the bulk uranium ore sample, the characteristic X-fluorescence information of the uranium ore is excited, and the fluorescence information is received by the cadmium telluride detector and shaped by the charge-sensitive preamplifier and pulse shaping amplifier. After amplification, it is converted into an energy spectrum for analysis by a digital multi-channel spectrometer; the computer analyzes the distance information of the laser rangefinder, uses the detection response of different detectors to X-fluorescence and the penetration ability of characteristic X-fluorescence information of different energies A coupling model of the dual detection structure was established to overcome the influence of the geometric effect caused by the uneven surface of the massive uranium ore on the characteristic X-fluorescence intensity of multiple elements in the sample, and to improve the analysis accuracy of the online X-fluorescence analyzer.
实施例1:Example 1:
1. 采用丹东东方电子管厂银靶X光管1,X光管高压2设置为80000伏,能有效地激发铀矿中多元素的特征X射线荧光; X光管l与样品14表面的距离为50毫米。1. The silver target X-ray tube 1 of Dandong Dongfang Electron Tube Factory is used, and the high voltage 2 of the X-ray tube is set to 80,000 volts, which can effectively excite the characteristic X-ray fluorescence of multi-elements in the uranium ore; the distance between the X-ray tube 1 and the surface of the
2. 采用美国amptek公司SDD-123硅漂移探测器3与样品表面之间夹角为90度,距离为6毫米,这些是为了保证分析仪获得较好的分辨率。2. The angle between the SDD-123
3. 采用美国amptek公司碲化镉探测器7与样品表面之间夹角为90度,距离为6毫米,这些是为了保证分析仪获得较好的分辨率。3. The angle between the cadmium telluride detector 7 and the surface of the sample is 90 degrees and the distance is 6 mm. These are to ensure that the analyzer can obtain better resolution.
4. 激发光源、探测系统与数字化多道谱仪11固定在5毫米的船型雪橇刮板,采用物理重力原理压平较大块状铀矿样品。4. The excitation light source, detection system and digital
5. 激光光源为上海倍乐的LOD红外激光器。激光光源发出红外光,激光光源发出红外光,照在样品台上,实时监测样品表面变化数据 。5. The laser light source is the LOD infrared laser of Shanghai Beile. The laser light source emits infrared light, and the laser light source emits infrared light, which shines on the sample stage to monitor the change data of the sample surface in real time.
6. 配置10kg的铀矿样品,样品测量100s。6. Configure a 10kg uranium ore sample and measure the sample for 100s.
7. 硅漂移探测器3收集的信号利用脉冲成型放大器6放大,之后经过数字化多道谱仪11转化为可用于分析的能谱图(如图2),再由计算机进行数据处理,得到中铀矿中低原子序数元素含量。7. The signal collected by the
8. 碲化镉探测器7收集的信号利用脉冲成型放大器6放大,之后经过数字化多道谱仪11转化为可用于分析的能谱图(如图3),再由计算机进行数据处理,得到中铀矿中高原子序数元素含量。8. The signal collected by the cadmium telluride detector 7 is amplified by the pulse shaping amplifier 6, and then converted into an energy spectrum that can be used for analysis by the digital multi-channel spectrometer 11 (as shown in Figure 3), and then the data is processed by the computer. The content of high atomic number elements in uranium ore.
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下还可以做出若干改进,这些改进也应视为本发明的保护范围。The above are only the preferred embodiments of the present invention. It should be pointed out that for those skilled in the art, several improvements can be made without departing from the principles of the present invention, and these improvements should also be regarded as the present invention. scope of protection.
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