Magnetic Deflector and Methods of Use Thereof
20240418662 ยท 2024-12-19
Inventors
Cpc classification
International classification
Abstract
Various examples are provided related to magnetic deflectors and their use in, e.g., proton-induced X-ray emission (PIXE) spectroscopy. In one example, a magnetic deflector includes first and second magnets separated by a gap; a ferromagnetic yoke surrounding the magnets, the yoke extending between a ferromagnetic front cover and rear cover, each including a canal extending through the cover; and a removable entrance aperture detachably attached to the front cover. The entrance aperture includes an opening aligned with the canal of the front cover to limit ions entering the magnetic deflector through the entrance aperture to a specified conical region. A direction of trajectory of an ion entering the magnetic deflector is altered by the magnetic field as it travels through the gap. The magnetic deflector can be used in a PIXE spectroscopy system to enable detection of low energy x-rays emitted from low-Z elements.
Claims
1. A magnetic deflector, comprising: first and second magnets extending substantially parallel to each other, the first and second magnets separated by a gap having a fixed distance, the first and second magnets establishing a magnetic field across the gap; a ferromagnetic yoke surrounding the first and second magnets, the yoke extending between a ferromagnetic front cover and a ferromagnetic rear cover, each of the front cover and the rear cover comprising a canal extending through the front and rear cover from an inner surface adjacent to the gap to an outer surface opposite the gap, the canals of the front and rear covers axially aligned with each other and the gap when the first and second magnets are enclosed within the yoke and front and rear covers; and a removable entrance aperture detachably attached to the front cover, the entrance aperture comprising an opening aligned with the canal of the front cover, the opening configured to limit ions entering the magnetic deflector through the entrance aperture to a specified conical region within the gap, where a direction of trajectory of an ion entering the magnetic deflector is altered by the magnetic field as it travels through the gap.
2. The magnetic deflector of claim 1, further comprising a plurality of alignment spacers configured to align the first and second magnets within the yoke, wherein the plurality of alignment spacers are nonmagnetic.
3. The magnetic deflector of claim 2, wherein the plurality of alignment spacers are positioned between the first and second magnets and sidewalls of the yoke to secure the first and second magnets in position without epoxy or adhesive.
4. The magnetic deflector of claim 2, wherein at least a portion of the plurality of alignment spacers are configured to maintain the fixed distance of the gap between the first and second magnets.
5. The magnetic deflector of claim 4, wherein individual alignment spacers of the at least a portion of the plurality of alignment spacers comprise a shoulder that maintains the fixed distance of the gap between the first and second magnets.
6. The magnetic deflector of claim 1, further comprising an isolating spacer adjacent to the outer surface of the rear cover, the isolating spacer configured to electrically isolate the magnetic deflector from a detector positioned adjacent to the rear cover.
7. The magnetic deflector of claim 6, wherein the isolating spacer is a Teflon spacer.
8. The magnetic deflector of claim 1, wherein the yoke comprises first and second portions having a U-shaped cross-section, wherein sidewalls of the first and second portions align to surround the first and second magnets.
9. The magnetic deflector of claim 1, wherein the front cover comprises a recess in the outer surface configured to receive the removable entrance aperture, the recess aligned with the canal extending through the front cover.
10. The magnetic deflector of claim 1, comprising a removable exit aperture detachably attached to the rear cover, the exit aperture comprising an opening aligned with the canal of the rear cover, the opening configured to limit ions exiting the magnetic deflector through the exit aperture.
11. The magnetic deflector of claim 10, wherein the opening of the exit aperture is substantially aligned with the opening of the entrance aperture.
12. The magnetic deflector of claim 1, comprising a mounting plate detachably attached to the rear cover.
13. The magnetic deflector of claim 1, wherein the magnetic field is substantially uniform along a length of the first and second magnets.
14. The magnetic deflector of claim 1, wherein the magnetic field is about 0.8 T or greater.
15. A proton-induced X-ray emission (PIXE) spectroscopy system, comprising: a proton source configured to direct a charged ion beam at a target in a vacuum chamber; an X-ray detector configured to detect X-ray emissions from the target; and a magnetic deflector positioned between the target and the X-ray detector; the magnetic deflector comprising: first and second magnets extending substantially parallel to each other, the first and second magnets separated by a gap having a fixed distance, the first and second magnets establishing a magnetic field across the gap; a ferromagnetic yoke surrounding the first and second magnets, the yoke extending between a ferromagnetic front cover and a ferromagnetic rear cover, each of the front cover and the rear cover comprising a canal extending through the front and rear cover from an inner surface adjacent to the gap to an outer surface opposite the gap, the canals of the front and rear covers axially aligned with each other and the gap when the first and second magnets are enclosed within the yoke and front and rear covers, and aligned with the X-ray detector; and a removable entrance aperture detachably attached to the front cover, the entrance aperture comprising an opening aligned with the canal of the front cover, the opening configured to limit ions entering the magnetic deflector through the entrance aperture to a specified conical region within the gap, where a direction of trajectory of an ion entering the magnetic deflector is altered by the magnetic field as it travels through the gap and a direction of X-rays passing through the magnetic deflector are not altered by the magnetic field.
16. The PIXE spectroscopy system of claim 15, wherein the magnetic deflector comprises a plurality of alignment spacers configured to align the first and second magnets within the yoke, wherein the plurality of alignment spacers are nonmagnetic.
17. The PIXE spectroscopy system of claim 16, wherein the plurality of alignment spacers are positioned between the first and second magnets and sidewalls of the yoke to secure the first and second magnets in position without epoxy or adhesive.
18. The PIXE spectroscopy system of claim 15, wherein the magnetic deflector comprises an isolating spacer adjacent to the outer surface of the rear cover, the isolating spacer configured to electrically isolate the magnetic deflector from a detector positioned adjacent to the rear cover.
19. The PIXE spectroscopy system of claim 15, wherein the magnetic deflector comprises a removable exit aperture detachably attached to the rear cover, the exit aperture comprising an opening aligned with the canal of the rear cover, the opening configured to limit ions exiting the magnetic deflector through the exit aperture.
20. The PIXE spectroscopy system of claim 19, wherein the opening of the exit aperture is substantially aligned with the opening of the entrance aperture.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] Many aspects of the present disclosure can be better understood with reference to the following drawings. The components in the drawings are not necessarily to scale, emphasis instead being placed upon clearly illustrating the principles of the present disclosure. Moreover, in the drawings, like reference numerals designate corresponding parts throughout the several views.
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DETAILED DESCRIPTION
[0027] Disclosed herein are various examples related to magnetic deflectors and their use in, e.g., proton-induced X-ray emission (PIXE) spectroscopy. A new technique has been developed which allows the detection and measurement of X-rays from light elements which can be particularly useful for biological applications. Reference will now be made in detail to the description of the embodiments as illustrated in the drawings, wherein like reference numbers indicate like parts throughout the several views.
[0028] Proton-induced X-ray emission (PIXE) spectroscopy is a long-established method of nondestructive elemental analysis for materials. PIXE has proven to be a reliable and sensitive technique for the detection and quantification of trace elements with atomic numbers in the range of 13-92. PIXE relies upon the relatively high probability that an energetic (1-3 MeV) ion (usually a proton) can undergo an inelastic collision with the electrons in an atom that results in the ionization of an inner-shell electron. The resulting vacancy will be filled by other electrons cascading from higher shells, releasing energy that can be emitted as one or more x-rays characteristic of the atom from which it originates. The physical process of PIXE is illustrated in
[0029] The need to detect low energy X-rays below 1 keV has led to the development of ultra-thin windows for use with a variety of X-ray detectors. The traditional Be window used for solid state X-ray detectors can be replaced with thinner, more X-ray transparent material such as polymer, graphenic carbon, diamond or silicon nitride. These new ultra-thin windows can allow for the detection of elements down to carbon and in some cases lithium while maintaining the detector's vacuum environment. With PIXE however, protons scattered from the sample backward into the detector can cause damage to the detector, thereby substantially reducing the detector lifetime. The energy released from each backscattered ion can overwhelm the detector's preamplifier as they travel through the detector, causing it to reset and increase system deadtime. These backscattered ions can damage the detector and entry window over time, drastically reducing its efficiency, resolution and overall lifetime.
[0030] The standard procedure to protect the detector the backscattered protons is to insert an absorber between the sample and the detector. With an absorber of appropriate thickness placed before the entry window, the backscattered ions can be effectively eliminated.
[0031] In order to enable the detection low energy x-rays and the subsequent quantification of low-Z elements in samples, a uniquely designed magnetic deflector 209 is utilized to deflect protons away from the detector 206 as shown in
Magnetic Deflector Design
[0032] Referring to
[0033] The front cover 309a and rear cover 309b include channels, passages or canals that extend through the covers to align with the gap between the magnets 303 thereby allowing x-rays to pass through the magnetic deflector 209. A removable entrance aperture 315 located in the front cover 309a limits the backscattered ions to a specific conical region. The dimensions of the entrance aperture 315 can be based upon the solid angle of the X-ray detector 206 or optional exit aperture 321. The radius of the entrance aperture 315 is calculated using the angle of half the solid angle's apex, the radius of the detector 206 or optional exit aperture 321 and its distance from the target location, and the distance of the entrance aperture 315 from the target location. As shown in
[0034]
[0035] The magnetic deflector 209 of
Magnetic Deflector Theory and Modeling
[0036] As an ion with an initial velocity, , traverses a magnetic field, B, the magnetic force acting on the ion causes it to travel in a circular motion perpendicular to B and in the plane of its
.
) traverses in a region with a length of z where the magnetic field,
, is perpendicular to the ion trajectory and directed out of the page.
[0037] The radius, r, of the circular path is defined by the equation:
where E is the sum of the ion beam energy and the ion rest energy, E.sub.0. B is the magnetic flux density perpendicular to ion's path of motion, q is the charge of the ion. and c is the speed of light in a vacuum, (310.sup.8 m/s). The radius of the ion's trajectory, length of the magnetic field region, z, and initial entry angle, , can be used to determine the amount of deflection, x, caused by the magnetic field. The equation derived for use in determining the deflection is:
[0038] Determining the magnetic flux density utilizes a different approach, as the value of B varies per location and can be influenced by the magnets and shape of the ferromagnetic yoke. For example, Finite Element Method Magnetics (FEMM) can be used to simulate the lateral cross-section of various designs to determine an optimal design which can produce a uniform magnetic field along the ion's travel path. FEMM is an open source software package which utilizes finite element analysis to solve 2D and axisymmetric electromagnetic and steady state heat flow problems.
[0039] Once the general design is decided upon, yoke thickness and spacing can be adjusted to maximize the magnetic flux density while allowing full use of the X-ray detector 206.
Magnetic Deflector Validation
[0040] A prototype magnetic deflector 206 was assembled and tested for validation of the design. The magnetic field strength was measured for comparison to the simulated values from FEMM. For this purpose, a benchtop test station was assembled using a small laser table, two linear manipulators, a T-slotted rail and miscellaneous hardware. A USB-ST1 Micromag USB Gauss Meter was used to measure the magnetic flux density. This single-axis gauss meter has a 22 mm.sup.2 detector with a 19,999 G range, 1 G resolution and 2% accuracy.
[0041] Proton Deflection. Backscattered proton deflection testing was conducted in the general purpose endstation of the National Electrostatic Corporation (NEC) 3 MV 9SH single-ended Pelletron. The experimental setup in the endstation chamber is shown in
[0042] As the detector mount restricted it to a distance located further away from the target than the X-ray detector 206, a detector 706 with a larger active area was chosen to ensure all backscattered protons could be detected. All targets 709 were mounted to a manual XYZ-stage. A thick silicon target 709 with a 240 nm gold layer and 70 nm intermediary titanium adhesion layer was chosen for testing. At a 135 scattering angle, gold has a kinematic factor of 0.9827. The incoming proton beam energy was set to 1.000 MeV for the initial test run and was increased by 100 keV for each subsequent run until the backscattered protons were no longer deflected. The beam energy was then reduced in 10 keV increments until the full deflection occurred again.
[0043] Light Element PIXE. In preparation for testing the light element PIXE system, the particle detector 706 after the magnetic deflector 209 was removed, and in its place, an Amptek 70 mm.sup.2 X-123 Fast silicon drift detector (SDD) X-ray detector 206 was mounted. The X-ray detector 206 was internally collimated to 50 mm.sup.2 and comes with Amptek's patented C2 entry window, which allowed for the transmission of lithium X-rays to the SDD. C2 windows were 40 nm thick silicon nitride windows with a 30 nm aluminum coating. The window was affixed to a 15 m thick hexagonal silicon grid which reduced the open area for X-ray transmission to 80% of the original. Control of the X-ray detector and data acquisition was handled by Amptek's DPPMCA Display and Acquisition Software. For testing purposes, no changes were made to the detector's default settings. With the magnetic deflector 209 in place, the X-ray detector 206 was 118.4 mm away from the targets, providing a solid angle of 3.59 msr. To maintain this solid angle, no adjustments along the Z-axis were made to the stage when positioning samples. Due to the entrance aperture and shielding provided by the deflector's yoke 306 and front cover 309a, all entering X-rays travel directly to the internally collimated active area of the detector 206. The energy of the proton beam was selected based on the results of the particle deflection tests.
[0044] A variety of organic and inorganic samples containing low-Z elements were studied to test the detection capabilities of the light element PIXE system of low energy (<1 keV) X-rays. A manganese oxide thick target of unknown chemical composition was used for confirming the ability to see oxygen and carbon from possible contaminants. It was also used in determining the detector resolution at 5.899 keV (Mn K) and 0.523 keV (O K) and setting the energy calibration for subsequent spectra. Once the ability to see elements below aluminum was confirmed, a sodium chloride crystal was analyzed to study the system's accuracy at determining the atomic ratios between elements within a sample. Sodium chloride was primarily chosen due to the importance of sodium in biological systems. A pressed pellet of D-(+)-glucose, the most abundant carbohydrate and source of energy in cell function, with a chemical formula of C.sub.6H.sub.12O.sub.6 was also analyzed as part of studying atomic ratios. As a complete test of the system, a section from a green hibiscus (Hibiscus rosa-sinenesis) leaf was analyzed, and its elemental concentrations were determined. The final sample investigated was a 10 m thick section of rat brain supported by a 2 m polycarbonate backing film. This was chosen due to previous analysis revealing no detectable trace elements above copper. The rat brain section was also analyzed using standard PIXE with the same beam energy and an 80 m thick carbon-filled polyethylene absorber for blocking backscattered particles. This was done to investigate and compare the differences in results between the two experimental setups.
Results and Discussion
[0045] Magnetic Flux Density.
[0046] The measured and simulated results for the centrally located longitudinal cross-section are presented in
[0047] The higher simulated results for the lateral and longitudinal cross-sections may be attributed to not accounting for manufacturing tolerances during simulation. The 15-21 m thickness of each magnet's nickel-copper-nickel plating was also neglected in the model, which may have contributed to the higher simulated magnetic flux density. During assembly, some of the corners of the magnets were slightly damaged, which could cause a reduction in magnetic flux density. Despite the difference between simulated and experimental results, FEMM still proved to be a useful aid in the design process of the magnetic deflector 209.
[0048] Proton Deflection. With an initial beam energy of 1.000 MeV, all backscattered protons entering the magnetic deflector were successfully steered away from the particle detector. This trend continued with each incremental beam energy increase of 100 keV up to 1.240 MeV.
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[0050] Light Element PIXE Analysis. A 1.000 MeV proton beam with a spot size of 0.25 mm.sup.2 was chosen for light element PIXE, and the average beam current was 1.50.5 nA. Data acquisition, spectra calibration, and determination of detector resolution were performed using Amptek's freely available DPPMCA display and acquisition software. The initial run on the manganese oxide target proved successful in detecting elements down to carbon.
[0051] A linear fit between the O and Mn K X-ray peaks was used for energy calibration of this and all subsequent spectra. Additionally, the linearity of the energy calibration was verified using K peaks identified in the other samples investigated in this work. A plot of the energy calibration curve for the X-ray detector is found in
[0052] When analyzing the sodium chloride crystal, the light element PIXE system could detect trace concentrations of boron (0.185 keV) without difficulty.
[0053] GeoPIXE 7.5r software was used for quantification of the spectrum, and the relative mass and atomic concentrations for all quantifiable elements are listed in Table 1. GeoPIXE was not designed to quantify any element below 0.200 keV, which prevented the determination of the amount of boron detected. Sodium and chlorine concentrations were very low given they were the primary elements in the target. The reduction in concentration is likely the result of ion beam induced luminescence of the target. The ultra-thin C2 window of the X-ray detector is not a light tight design. Thus, the light emitted from the target during ion beam interaction overwhelms the detector, causing it to reset more frequently while preventing it from processing incoming X-rays. Despite this issue and the presence of other contaminants, the atomic ratio of sodium to chlorine is 0.97:1, which is within the range of uncertainty.
TABLE-US-00001 TABLE 1 Mass and atomic concentration of elements found in NaCl crystal. Mass Concentration Atomic Concentration Detection Detection Concentration Uncertainty Limits Concentration Uncertainty Limits Element (ng/mg) (ng/mg) (ng/mg) (mol/mol) (mol/mol) (mol/mol) C 1320 60 40 6420 270 190 O 79 6 9 289 22 31 Na 202 8 2 510 20 6 Cl 321 9 4 529 15 6
[0054] Issues arose when analyzing the pressed pellet of D-(+)-Glucose. The pellet was found to be insulating at the beginning of the first of two runs performed on it, with it charging up and arcing during the run. As the initial run progressed, the pellet became more conductive as a dark, carbonized layer formed on the surface where the proton beam was irradiating it. Once the first run was completed, a follow-up run was performed, which showed a reduction in background caused by the sample charging up. There was also a noticeable reduction in oxygen, while the amount of carbon appeared to increase.
[0055] While charge was collected for 2 C for both data runs, the insulative nature and charging up of the sample interjected a large margin of error into the charge integration. To overcome this, the RBS spectra were analyzed, and the correct charge for each spectrum was extracted. With the correct charge obtained, elemental concentrations were extracted and the ratio of carbon to oxygen was determined for each run and are listed in Table 2. It was confirmed that the sample pellet of D-(+)-Glucose likely began to lose oxygen as the beam of protons interacted with the sample and began breaking molecular bonds. This resulted in change in the carbon to oxygen ratio from 1:1 to 3:1.
TABLE-US-00002 TABLE 2 Comparison of atomic concentration of elements in D-(+)- Glucose sample and C to O ratio for each run performed. Run 1 Run 2 Concentration Concentration Element (mmol/mol) (mmol/mol) C 1470 2150 O 520 270 Al 0.76 0.77 C to O 3 8 Ratio
[0056] During the second run, the ratio increased to 8:1, while the relative concentration of carbon increased by 677,592 mol/mol. This is potentially from free carbon in the vacuum chamber collecting on the surface. Additionally, the concentration for the second run is artificially high due to the use of identical target information in the yield files for each run which did not account for prior elemental loss. While not the focus of this work, it presents a possible use case for measuring elemental concentration loss due to the release of volatiles from ion beam interaction over time. The loss of volatiles in subsequent organic samples was not investigated at this time as the focus was on showing the functionality of the magnetic deflector system.
[0057] Prior to analysis, the green hibiscus leaf sample was cleaned using DI water and shade dried for 4-5 days to retain the nutrient value. A small section was cut off and mounted on the sample holder. The leaf sample presented less of an issue compared to the glucose sample, although small hair like protrusions called trichomes would luminesce when exposed to the ion beam. Adjusting the sample position resolved this issue and charge collection was not impacted.
[0058] The relative concentrations of detected elements can be found in Table 3. For the purposes of this test, cellulose (C.sub.6H.sub.10O.sub.5) was used for the matrix composition of the leaf sample. Uniform density and thickness were assumed. Because of the presence of carbon, nitrogen, oxygen, sodium and magnesium, the leaf sample proved to be a good sample to showcase the capabilities of the light element PIXE system.
TABLE-US-00003 TABLE 3 Elemental concentrations of analyzed region of the green hibiscus leaf sample. Detection Concentration Uncertainty Limits Element (ng/mg) (ng/mg) (ng/mg) C 160200 1200 20 N 1750 250 90 O 27400 600 30 Na 3540 90 8 Mg 571 22 7 Si 40 3 4 P 735 9 6 S 1625 21 9 Cl 1546 25 10 K 5970 130 11 Ca 1420 30 15 Mn 48 18 24
[0059] A comparison between a standard PIXE run with an 80 m thick carbon-filled polyethylene absorber and a light element PIXE run on the 10 m thick rat brain slice is shown in
[0060] Similarly, a comparison between elemental concentrations obtained from both methods is available in Table 4. With the absorber in place, standard PIXE is shown to be theoretically capable of detecting sodium and magnesium, but the detection limit, or minimum detectable limit (MDL), for each far exceeded the amount present in the sample, which was detected with light element PIXE. Concentrations of silicon and aluminum showed a large discrepancy between the different setups, while calcium and iron were very similar for both. Phosphorus, sulfur, chlorine, and potassium varied between the two setups, but elemental ratios between them showed similar trends in their individual runs.
TABLE-US-00004 TABLE 4 Comparison between concentrations obtained from standard PIXE and light element PIXE of a rat brain sliced tissue sample. Standard PIXE with 80 m C-filled Light Element PIXE with Magnetic Polyethylene Absorber Deflector Detection Detection Concentration Uncertainty Limits Concentration Uncertainty Limits Element (ng/mg) (ng/mg) (ng/mg) (ng/mg) (ng/mg) (ng/mg) C 141000 2000 8 N 52000 2000 40 O 62700 1500 27 F 2480 210 16 Na <MDL 40000 70000 1830 90 6 Mg <MDL 250 500 316 11 5 Al 100 30 50 37 2 5 Si 111 12 15 15 3 4 P 6180 70 11 5040 110 6 S 2620 40 10 1790 50 7 Cl 2950 40 8 2180 40 8 K 9020 70 6 6240 140 8 Ca 158 11 8 167 9 9 Fe 91 15 23 87 22 24
[0061] The differences in elemental concentrations between experimental runs can be attributed to repeatability of sample positioning. Although the intention was to analyze the same location for both experimental runs, it should be noted that setup between each run needed moving the sample out of position. While the sample was moved as close to the same position as possible, several factors limited exact repositioning to within 3010 m. Poor camera resolution, stage repeatability and beam drift are major limiting factors affecting the reanalysis of the same location. Additionally, elemental composition can drastically change in the rat brain tissue over distances >20 m, which is not a trivial distance for beam spot sizes of <1 mm.sup.2. As such, a variation in the elemental composition between these experimental runs was expected.
[0062] A prototype magnetic deflector capable of deflecting 1.219 MeV backscattered protons was developed for a light element PIXE system. Several samples were analyzed to test the system and determine its usefulness. The system was found to be capable of detecting elements down to boron in samples, allowing for a nondestructive method of determining the concentration of light elements with a short setup time and run times comparable to standard PIXE for heavier elements. This makes it ideally suited for biological applications involving the study of low-Z elements within very thin or thick, homogenous samples primarily composed of light elements. It is also well suited for investigating surface contamination of trace low-Z elements on a variety of other sample types. The magnetic deflector can be reduced in size for use in a light ion microprobe, and better materials with higher magnetic saturation can be utilized with the yoke.
[0063] It should be emphasized that the above-described embodiments of the present disclosure are merely possible examples of implementations set forth for a clear understanding of the principles of the disclosure. Many variations and modifications may be made to the above-described embodiment(s) without departing substantially from the spirit and principles of the disclosure. All such modifications and variations are intended to be included herein within the scope of this disclosure and protected by the following claims.
[0064] The term substantially is meant to permit deviations from the descriptive term that don't negatively impact the intended purpose. When not otherwise defined, substantially can mean within a variation of 20% or less. Descriptive terms are implicitly understood to be modified by the word substantially, even if the term is not explicitly modified by the word substantially.
[0065] It should be noted that ratios, concentrations, amounts, and other numerical data may be expressed herein in a range format. It is to be understood that such a range format is used for convenience and brevity, and thus, should be interpreted in a flexible manner to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. To illustrate, a concentration range of about 0.1% to about 5% should be interpreted to include not only the explicitly recited concentration of about 0.1 wt % to about 5 wt %, but also include individual concentrations (e.g., 1%, 2%, 3%, and 4%) and the sub-ranges (e.g., 0.5%, 1.1%, 2.2%, 3.3%, and 4.4%) within the indicated range. The term about can include traditional rounding according to significant figures of numerical values. In addition, the phrase about x to y includes about x to about y.