ASTM E387-04(2014)

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 manufacturer’s literature represents the performance of a new instrument, tested exactly in accordance with the manufacturer’s specification. The implication is that the manufacturer’s stated SRPR can serve as a benchmark for future performance, provided that the user performs the manufacturer’s 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., (4) show that its results tend to correlate well with those of the specified wavelength method, but for critical comparison with the manufacturer’s specification, the method used by the manufacturer must be used. Because some instruments reduce SRP by incorporating moderately narrow bandpass SRP-blocking filters that are changed as the wavelength range is scanned, it is possible for SRPR determinations to be highly inaccurate if the cutoff wavelength of the SRP filter falls too close to the absorption edge of an instrument’s SRP-reducing filter 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.

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.

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 and health practices and determine the applicability of regulatory limitations prior to use.