Índice de Refração - D-1218
Índice de Refração - D-1218
Índice de Refração - D-1218
1. Scope
1.1 This test method covers the measurement of refractive
index, accurate to four decimal places or better, of transparent
and light-colored hydrocarbons in the range of 1.3300 to
1.5000 at temperatures from 20 to 30C by manual (opticalmechanical) or automatic (digital) procedure.
1.2 The manual (optical-mechanical) procedure also covers
the measurement of refractive dispersion accurate to the fourth
decimal place or better.
D 1500 Test Method for ASTM Color of Petroleum Products (ASTM Color Scale)
D 6299 Practice for Applying Statistical Quality Assurance
Techniques to Evaluate Analytical Measurement System
Performance
D 6300 Practice for Determination of Precision and Bias
Data for Use in Test Methods for Petroleum Products and
Lubricants
E 1 Specification for ASTM Liquid-in-Glass Thermometers
2.2 ASTM Adjuncts:
Determination of Precision and Bias Data for Use in Test
Methods for Petroleum Products and Lubricants, Version
4.0.653
NOTE 1The test method may be suitable for measuring the refractive
indices of liquids above 1.5000 and at temperatures both below 20C and
above 30C; however, the test method precision may not apply. Verification of the accuracy of such measurements will depend upon the
availability of reliable, certified reference standards that demonstrate the
performance of the instrument used under the particular measuring
conditions.
1.3 The test method may not be applicable to liquids that are
strongly colored, or that have bubble points so near the test
temperature that a reading cannot be obtained before substantial weathering takes place. Liquid color should be limited to
No. 4 ASTM Color or lighter, as determined by Test Method
D 1500.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards: 2
D 1193 Specification for Reagent Water
3
Available from ASTM International Headquarters. Order No. ADJD6300.
(Originally published as Lawrey, D. M. G., ed., Calculation of Precision Data:
Petroleum Test Methods, ASTM International, 1996.)
Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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3. Terminology
3.1 Definitions:
3.1.1 refractive dispersionthe difference between the refractive indexes of a substance for light of two different
wavelengths, both indexes being measured at the same temperature. For convenience in calculations, the value of the
difference thus obtained is usually multiplied by 10 000.
3.1.2 refractive indexthe ratio of the velocity of light (of
specified wavelength) in air, to its velocity in the substance
under examination. It may also be defined as the sine of the
angle of incidence divided by the sine of the angle of
refraction, as light passes from air into the substance. This is
the relative index of refraction. If absolute refractive index
(that is, referred to vacuum) is desired, this value should be
multiplied by the factor 1.00027, the absolute refractive index
of air. The numerical value of refractive index of liquids varies
inversely with both wavelength and temperature.
D 1218 02 (2007)
facturer will recommend and supply a suitable filter or adapt a
commercially-available filter (for example, interference filter)
to suit the application.
6. Apparatus
6.1 Refractometer, high-resolution optical-mechanical refractometer of the Abbe type with suitable measuring range
(1.3300 to 1.5000 or higher) and an accuracy/resolution of
0.0001 or better refractive index.
NOTE 2Prior to 2001, Test Method D 1218 was based on a Bausch &
Lomb Refractometer. However, this instrument is no longer manufactured.
Currently available manual refractometers are of the Abbe type (critical
angle refractometers, see X1.2.3). There is a variety of refractometers that
have been found to be suitable for this measurement. Some instruments
offer a wider measuring range but it is important to verify the uniformity
of accuracy across the entire measuring range and to ensure suitable
calibration materials are available for this verification.
6 0.1C
6 0.1C
0.1C or better
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8. Sampling
8.1 A sample of at least 0.5 mL is required. The sample shall
be free of suspended solids, water, or other materials that may
settle onto the prism surface and affect the measured reading.
Water can be removed from hydrocarbons by treatment with
calcium chloride followed by filtering or centrifuging to
remove the desiccant. The possibility of changing the composition of the sample by action of the drying agent, by selective
adsorption on the filter, or by fractional evaporation, shall be
considered. (WarningVolatile hydrocarbon samples are
flammable.)
9. Preparation of Apparatus
9.1 The refractometer shall be kept scrupulously clean at all
times. Dust and oil can impair the optical component of the
instrument. Thoroughly clean the prism faces with toluene,
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D 1218 02 (2007)
12.5 Following manufacturers instructions, make any additional adjustment until the sharp boundary line intersects the
midpoint of the crosshairs superimposed on the field.
12.6 Read the refractive index on the scale. Repeat 12.5 at
least four times, approaching from either side of the sharp
boundary line, and average the scale readings.
12.7 Record and report the average refractive index value.
12.8 If instrument is capable of determining refractive
dispersion, change the light source to a light source with
different wavelength. Determine the refractive index at the
secondary wavelength following 12.4-12.7.
followed by n-pentane (see Note 4) (WarningThese materials are extremely flammable. Harmful if inhaled. Vapors may
cause flash fire.) using cotton swabs, fresh clean lens tissue, or
similar material, in accordance with manufacturers instructions. Do not dry the prism faces by rubbing with dry cotton.
9.2 Adjust the thermostat bath/circulator settings or the
electronic temperature control system so that the temperature
indicated by the refractometer temperature measuring device is
within 0.1C of the desired value. Turn on the light source and
allow the refractometer to equilibrate for 30 min.
NOTE 6The constancy of the prism temperature can be seriously
affected by variations in ambient conditions such as air drafts or changes
in room temperature. Reasonable precautions should be taken to minimize
these factors.
(2)
12. Procedure
12.1 Ensure that the prism faces are clean and dry. Check
that the prism temperature is within 0.1C of the desired
temperature.
12.2 Unlock (if necessary) and open the prism assembly.
12.3 Place one or two drops of the sample on the lower
prism face. Close the prism assembly and lock (if necessary).
Turn on the light source. Allow 3 min temperature equilibration
time.
12.4 Look through the eyepiece and observe the field
consisting of a light and dark portion. Follow manufacturers
instructions to adjust the instrument so that the boundary
between the light and dark portions of the field is as sharp as
possible.
4
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: D02-1493.
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(1)
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D 1218 02 (2007)
21. Procedure
21.1 Ensure that the prism and the surrounding plate and
dish/plate (and presser, if fitted) are thoroughly cleaned as in
9.1. Ensure the prism temperature is correct and the instrument
has been properly calibrated.
21.2 Introduce the test sample to the prism ensuring that the
prism is adequately covered. Do not introduce an excessive
amount because this can slow the thermal equilibration. Lower
the sample presser (if fitted).
21.3 Take a succession of readings, noting values, until a
steady value is obtained. Record or report, or both, this value
as the refractive index of the sample at the test temperature.
(3)
(4)
NOTE 8From experience using the instrument, the user will be able to
judge with a safe margin the amount of time needed for a sample to
thermally equilibrate on the prism. Based on this, it may be possible on
some models to set an automatic delay time for readings. This enables a
fixed measuring time to be written in to the experimental protocol.
NOTE 9When successive readings are drifting, the direction of drift
will indicate what is happening to the sample. An upward drift means the
sample is cooling on the prism; a downward drift means the sample is
warming up. This is particularly noticeable when samples are much hotter
or cooler than the prism.
16. Apparatus
16.1 RefractometerAutomatic digital refractometer with a
suitable measuring range of 1.3300 to 1.5000 or higher,
capable of displaying the measured refractive index automatically and digitally. The instrument shall incorporate a solventresistant prism seal.
16.2 Temperature Control UnitSee 6.2.
16.3 Temperature Measuring DeviceA platinum resistance probe or equivalent. The accuracy and resolution of the
temperature measuring device shall be 0.1C or better.
16.4 Light SourceFiltered white light such as that obtained using a tungsten-halogen lamp or a light emitting diode
(LED), capable of providing the sodium D spectral line at 589
nm.
16.5 Light FiltersSee 6.5.
23. Report
23.1 An automatic digital electronic refractometer shall
provide a direct and digital reading of refractive index. This
can be manually recorded or, if the refractometer is equipped
with a computer interface, readings can be sent to a printer or
to a computer.
23.2 Report the refractive index to four decimal places and
the test temperature, for example:
nD 5 x.xxxx at 20C or n589 5 x.xxxx at 20C
rautomatic 5 0.0002
(6)
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(5)
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D 1218 02 (2007)
Rautomatic 5 0.0005
(7)
25. Keywords
APPENDIXES
(Nonmandatory Information)
X1. FACTORS THAT AFFECT PRECISION AND ACCURACY
can utilize a white light source, but often these instruments are
limited in accuracy because of the light source. High accuracy
Abbe refractometers require a pure spectral light source such as
a sodium arc lamp (see 6.4).
X1.2.4 Modern electronic digital refractometers function at
a single wavelength, invariably that of sodium light (589 nm).
The refractive index at this wavelength is denoted as nD.
X1.2.5 One of two types of light source tends to be used in
digital refractometers: (1) filtered white light source such as
that obtained using a tungsten-halogen lamp, or (2) light
emitting diode (LED).
X1.2.6 With both types of light source, the wavelength is
not a single value but is a narrow band spanning typically 10
nm or more about the nominal value (589 nm). The degree of
impurity (band width) will cause a dispersion of the detected
light from the sample. Instrument software can be used to
compensate for and thus minimize this error source but it will
nevertheless be a factor in determining the limiting accuracy of
the instrument. The dispersion error will however differ according to the substance measured. This is why instrument
manufacturers may specify the instrument accuracy as typically
or better than in order to cover a broad application scope.
X2.3 An optical-mechanical instrument may require calibration at only one point on the scale. Automatic digital
refractometers may require a single (zero), two-point, or
multi-point calibration. For each calibration a suitable calibration standard should be used.
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D 1218 02 (2007)
X2.4 The frequency of calibration will depend upon a
number of factors. When an electronic instrument is first
switched on and the liquid bath circulation is started, a period
of thermal adjustment is required to allow the internal environment, and particularly the optical system, to adjust to the
new condition. Calibration should not take place until the
instrument is in a steady-state. Experience will demonstrate
that this may be typically up to an hour. Similarly, if the
circulating liquid temperature is changed, a new calibration
sequence will be required. In circumstances where the instrument is used continuously and in a constant thermal condition,
the need for recalibration should be minimal.
X4.1 The performance of the instrument or the test procedure should be confirmed by analyzing a quality control (QC)
sample.
X4.2 It is recommended that the QC sample be representative of the material routinely analyzed. However, pure
materials may be used, if so desired. An ample supply of QC
sample material should be available for the intended period of
use, and should be homogeneous and stable under the anticipated storage conditions.
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D 1218 02 (2007)
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