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Standard Test Method for Estimating Stray Radiant Power Ratio of Dispersive Spectrophotometers by the Opaque Filter Method
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NORM herausgegeben am 1.11.2022
Bezeichnung normen: ASTM E387-04(2022)
Ausgabedatum normen: 1.11.2022
SKU: NS-1088761
Zahl der Seiten: 11
Gewicht ca.: 33 g (0.07 Pfund)
Land: Amerikanische technische Norm
Kategorie: Technische Normen ASTM
Keywords:
molecular spectroscopy, spectrophotometry, SRP, SRPR, stray light, stray radiant power, stray radiant power ratio,, ICS Number Code 17.180.30 (Optical measuring instruments)
Significance and Use | ||||
5.1?Stray radiant power can be a significant source of error in spectrophotometric measurements. SRP usually increases with the passage of time; therefore, testing should be performed periodically. Moreover, the SRPR test is an excellent indicator of the overall condition of a spectrophotometer. A control-chart record of the results of routinely performed SRPR tests can be a useful indicator of need for corrective action or, at least, of the changing reliability of critical measurements. 5.2?This test method provides a means of determining the stray radiant power ratio of a spectrophotometer at selected wavelengths in a spectral range, as determined by the SRP filter used, thereby revealing those wavelength regions where significant photometric errors might occur. It does not provide a means of calculating corrections to indicated absorbance (or transmittance) values. The test method must be used with care and understanding, as erroneous results can occur, especially with respect to some modern grating instruments that incorporate moderately narrow bandpass SRP-blocking filters. This test method does not provide a basis for comparing the performance of different spectrophotometers. Note 8:?Kaye 5.3?This
test method describes the performance of a spectrophotometer in
terms of the specific test parameters used. When an analytical
sample is measured, absorption by the sample of radiation outside
of the nominal bandpass at the analytical wavelength can cause a
photometric error, underestimating the transmittance or
overestimating the absorbance, and correspondingly underestimating
the SRPR.
5.4?The SRPR indicated by this test method using SRP filters is almost always an underestimation of the true value (see 1.3). A value cited in a manufacturers literature represents the performance of a new instrument, tested exactly in accordance with the manufacturers specification. The implication is that the manufacturers stated SRPR can serve as a benchmark for future performance, provided that the user performs the manufacturers specified test. It is recommended that users test new instruments promptly, thereby establishing a comparative benchmark in terms of their own testing facilities. The solution filter ratio method (4.3) is a convenient method for control-charting SRPR. Mielenz, et al., 1.1?Stray radiant power (SRP) can be a significant source of error in spectrophotometric measurements, and the danger that such error exists is enhanced because its presence often is not suspected Note 1:?Research 1.2?These procedures are neither all-inclusive nor infallible. Because of the nature of readily available filter materials, with a few exceptions, the procedures are insensitive to SRP of very short wavelengths in the ultraviolet, or of lower frequencies in the infrared. Sharp cutoff longpass filters are available for testing for shorter wavelength SRP in the visible and the near infrared, and sharp cutoff shortpass filters are available for testing at longer visible wavelengths. The procedures are not necessarily valid for spike SRP nor for nearby SRP. (See Annexes for general discussion and definitions of these terms.) However, they are adequate in most cases and for typical applications. They do cover instruments using prisms or gratings in either single or double monochromators, and with single and double beam instruments. Note 2:?Instruments with array detectors are inherently prone
to having higher levels of SRP. See Annexes for the use of filters
to reduce SRP.
1.3?The proportion of SRP (that is, SRPR) encountered with a well-designed monochromator, used in a favorable spectral region, typically is 0.1 % transmittance or better, and with a double monochromator it can be less than 1?10-6, even with a broadband continuum source. Under these conditions, it may be difficult to do more than determine that it falls below a certain level. Because SRP test filters always absorb some of the SRP, and may absorb an appreciable amount if the specified measurement wavelength is not very close to the cutoff wavelength of the SRP filter, this test method underestimates the true SRPR. However, actual measurement sometimes requires special techniques and instrument operating conditions that are not typical of those occurring during use. When absorption measurements with continuum sources are being made, it can be that, owing to the effect of slit width on SRP in a double monochromator, these test procedures may offset in some degree the effect of absorption by the SRP filter; that is, because larger slit widths than normal might be used to admit enough energy to the monochromator to permit evaluation of the SRP, the stray proportion indicated could be greater than would normally be encountered in use (but the net effect is still more likely to be an underestimation of the true SRPR). Whether the indicated SRPR equals or differs from the normal-use value depends on how much the SRP is increased with the wider slits and on how much of the SRP is absorbed by the SRP filter. What must be accepted is that the numerical value obtained for the SRPR is a characteristic of the particular test conditions as well as of the performance of the instrument in normal use. It is an indication of whether high absorbance measurements of a sample are more or less likely to be biased by SRP in the neighborhood of the analytical wavelength where the sample test determination is made. 1.4?The principal reason for a test procedure that is not exactly representative of normal operation is that the effects of SRP are magnified in sample measurements at high absorbance. It might be necessary to increase sensitivity in some way during the test in order to evaluate the SRP adequately. This can be accomplished by increasing slit width and so obtaining sufficient energy to allow meaningful measurement of the SRP after the monochromatic energy has been removed by the SRP filter. However, some instruments automatically increase sensitivity by increasing dynode voltages of the photomultiplier detector. This is particularly true of high-end double monochromator instruments in their ultraviolet and visible ranges. A further reason for increasing energy or sensitivity can be that many instruments have only absorbance scales, which obviously do not extend to zero transmittance. Even a SRP-proportion as large as 1 % may fall outside the measurement range. Note 3:?Instruments that have built-in optical attenuators to
balance sample absorption may make relatively inaccurate
measurements below 10 % transmittance, because of poor attenuator
linearity. The spectrophotometer manufacturer should be consulted
on how to calibrate transmittance of the attenuator at such lower
level of transmittance.
1.5?High accuracy in SRP measurement is not always required; a measurement reliable within 10 or 20 % may be sufficient. However, regulatory requirements, or the needs of a particular analysis, may require much higher accuracy. Painstaking measurements are always desirable. 1.6?The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.7?This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.8?This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. |
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2. Referenced Documents | ||||
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