An American National Standard

Designation: D 1747 – 99 (Reapproved 2004)e1

Standard Test Method for

Refractive Index of Viscous Materials1
This standard is issued under the fixed designation D 1747; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

e1 NOTE—Warning notes were editorially moved into the standard text in May 2004.

1. Scope D 1218 Test Method for Refractive Index and Refractive

1.1 This test method covers the measurement of refractive Dispersion of Hydrocarbon Liquids
indexes, accurate to two units in the fourth decimal place, of D 1500 Test Method for ASTM Color of Petroleum Prod-
transparent and light-colored viscous hydrocarbon liquids and ucts (ASTM Color Scale)
melted solids that have refractive indexes in the range between E 1 Specification for ASTM Liquid-in-Glass Thermometers
1.33 and 1.60, and at temperatures from 80 to 100°C. Tem- 3. Terminology
peratures lower than 80°C can be used provided that the
melting point of the sample is at least 10°C below the test 3.1 Definition:
temperature. 3.1.1 refractive index—the ratio of the velocity of light (of
1.2 This test method is not applicable, within the accuracy specified wavelength) in air, to its velocity in the substance
stated, to liquids having colors darker than ASTM Color No. 4, under examination. The relative index of refraction is defined
ASTM color as determined by Test Method D 1500, to liquids as the sine of the angle of incidence divided by the sine of the
which smoke or vaporize readily at the test temperature, or to angle of refraction, as light passes from air into the substance.
solids melting within 10°C of the test temperature. If absolute refractive index (that is, referred to vacuum) is
desired, this value should be multiplied by the factor 1.00027,
NOTE 1—The instrument can be successfully used for refractive indices the absolute refractive index of air. The numerical value of
above 1.60; but since certified liquid standards for ranges above 1.60 are
refractive index of liquids varies inversely with both wave-
not yet available, the accuracy of measurement under these conditions has
not been evaluated. length and temperature.
1.3 The values stated in SI units are to be regarded as 4. Summary of Test Method
standard. The values stated in inch-pound units are for infor- 4.1 The refractive index normally is measured by the critical
mation only. angle method using monochromatic light from a sodium lamp.
1.4 This standard does not purport to address all of the The instrument is previously adjusted by means of calibration
safety concerns, if any, associated with its use. It is the obtained with certified liquid standards.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5. Significance and Use
bility of regulatory limitations prior to use. 5.1 Refractive index is a fundamental physical property that
can be used in conjunction with other properties to characterize
2. Referenced Documents
pure hydrocarbons and their mixtures.
2.1 ASTM Standards: 2 5.2 The use of refractive index in correlative methods for
D 362 Specification for Industrial Grade Toluene3 the determination of the gross composition of viscous oils and
D 841 Specification for Nitration Grade Toluene waxes often requires its measurement at elevated temperatures.
6. Apparatus
1
This test method is under the jurisdiction of ASTM Committee D02 on 6.1 Refractometer, precision Abbé-type,4 having a range in
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee refractive index from 1.30 to 1.63. Other instruments reading
D02.04 on Hydrocarbon Analysis.
Current edition approved May 1, 2004. Published May 2004. Originally to at least four decimal places may be used.
approved in 1960. Last previous edition approved in 1999 as D 1747 – 99.
2
For referenced ASTM standards, visit the ASTM website, [Link], or
contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM
4
Standards volume information, refer to the standard’s Document Summary page on The Abbé-type precision refractometer is no longer available but may be
the ASTM website. obtainable from instrument exchanges or used equipment suppliers. Other precision
3
Withdrawn. refractometers may be suitable, but they have not as yet been tested cooperatively.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 D 1747 – 99 (2004)e1
TABLE 1 Primary Liquid Standards inhaled. High concentration can cause unconsciousness or
Certified Standard
Approximate Refractive Index, death. Contact can cause skin irritation and dermatitis.)
nD 7.2 Toluene, conforming to Specification D 362 or Specifi-
n-Hexadecane 1.41 cation D 841. (Warning—Flammable. Vapor harmful.)
trans-Decahydronaphthalene 1.44
1-Methylnaphthalene 1.59 8. Reference Standards
8.1 Primary Liquid Standards—Organic liquids listed in
Table 1, with the values of their refractive indexes for the
NOTE 2—When other instruments are used, follow the manufacturer’s sodium D line certified at 20, 25, 30, 80, and 100°C.6
instructions for operation, maintenance, calibration, and analysis. For (Warning—Primary standards are combustible.)
accepting the instrumentation for use, analysis of an NIST traceable
certified material to ensure accuracy should be performed.
8.2 Working Standards—For working standard hydrocar-
bons, reasonably well purified samples of n-hexadecane, trans-
6.2 Thermostat and Circulating Pump, capable of maintain- decahydronaphthalene, and 1-methylnaphthalene may be used.
ing the indicated prism temperature constant within 0.02°C. Their exact values are determined by comparison with standard
The circulating fluid consists of ethylene glycol or a mixture of samples of the same hydrocarbons having certified values of
30 to 40 volume % of glycerin in water flowing through the refractive index. (Warning—Working standards are combus-
prisms at a fixed rate of at least 2.5 L/min. For work at 100°C, tible.)
properly controlled wet steam is also suitable.
9. Sample
NOTE 3—The constancy of the prism temperature can be seriously
affected by variations in ambient conditions, such as air drafts or changes 9.1 A sample of at least 0.5 mL is required. The sample shall
in room temperature. Reasonable precautions should be taken to minimize be free of suspended solids, water, or other materials that tend
these factors. Insulation placed on the thermostat, circulating fluid lines, to scatter light. Water can be removed from hydrocarbons by
and refractometer also may prove to be helpful. treatment with calcium chloride followed by filtering or
6.3 Thermometers, conforming to Thermometer 21C for centrifuging to remove the desiccant. The possibility of chang-
determinations at 80°C or Thermometer 22C for determina- ing the composition of a sample by action of the drying agent,
tions at 100°C as given in Specification E 1 are recommended. by selective adsorption on the filter, or by fractional evapora-
The temperature measuring device, suitably calibrated, shall be tion, shall be considered.
positioned to measure the temperature of the prism (see Note 4)
within an appropriate holder. The holder shall provide for 10. Preparation of Apparatus
adequate immersion of the temperature measuring device and 10.1 The refractometer shall be kept scrupulously clean at
for free flow of the circulating fluid. The temperature measur- all times. Dust and oil, if allowed to accumulate on any part of
ing device holder assembly shall be insulated with a suitable the instrument, will find its way into the moving parts, causing
material, such as cork. wear and eventual misalignment. If permitted to collect on the
prism, dust will dull the polish, resulting in hazy lines.
NOTE 4—In the precision Abbé type refractometer, the thermostating
10.2 Thoroughly clean the prism faces with fresh clean lens
liquid should pass the thermometer on leaving, not on entering, the prism
assembly. tissue or surgical grade absorbent cotton saturated with a
suitable solvent. Pass the swab very lightly over the surface
6.4 Thermocouple, 5 copper-constantan foil type, 0.013-mm until it shows no tendency to streak. Repeat the procedure with
(0.0005-in.) thickness, and precision potentiometer. The ther- a fresh swab and solvent until both the glass and adjacent
mocouple is calibrated by immersing to a depth of 25 mm (1 polished metal surfaces are clean. Do not dry the prism faces
in.) in a circulating liquid thermostat and comparing with a by rubbing with dry cotton.
thermometer of known accuracy. 10.3 Adjust the thermostat so that the temperature as indi-
6.5 Light Source, Sodium Arc Lamp—The light source shall cated by the thermocouple inserted between the prism faces
be a sodium arc lamp, which shall be used only after the and wet with oil is within 0.2°C of the desired test temperature.
removal of Amici compensating prisms, if there are any present This temperature is to be held constant to within 0.02°C during
in the instrument. the test. Observe and record the thermometer reading corre-
NOTE 5—If the field division as observed in 12.2 shifts when the Amici sponding to the test temperature. Turn on the sodium arc lamp
prism is rotated, the prism should be removed to avoid incorrect readings. and allow it to warm up for 30 min.
7. Solvents 11. Standardization with Reference Liquids
7.1 Cleaning Solvent, any suitable solvent capable of clean- 11.1 Introduce a sample of the API Standard trans-
ing the apparatus as described in Section 10. 1,1,1, Trichloro- decahydronaphthalene to the prism which is adjusted to the
ethane has been found suitable to use. (Warning—Harmful if chosen test temperature of 80 or 100°C, turn the telescope
adjustment screw until a refractive index scale reading corre-
sponding to the certified refractive index for trans-
5
The sole source of supply of the apparatus known to the committee at this time decahydronaphthalene is observed, and adjust the instrument
is RdF Corp., 23 Elm Avenue, Hudson, NH 03051. If you are aware of alternative
suppliers, please provide this information to ASTM International Headquarters.
6
Your comments will receive careful consideration at a meeting of the responsible Available from API Standard Reference Office, Carnegie-Mellon University,
technical committee 1, which you may attend. Pittsburgh, PA 15213.

2
 D 1747 – 99 (2004)e1
according to the instructions given by the manufacturer until 11.6.4 Fluctuations in ambient temperatures should be mini-
the sharp boundary between the light and dark portions of the mized as much as possible during the test.
field passes through the intersection of the cross hairs of the
telescope. 12. Procedure
11.2 Check the accuracy of this setting by loading a fresh 12.1 Thoroughly clean the prism faces as described in 10.2.
sample of trans-decahydronaphthalene and measure its refrac- Adjust the thermostat so that the temperature indicated by the
tive index at the test temperature following the procedure thermocouple placed between the faces of the closed prism
described in Section 12. If the value for the refractive index (loaded with oil) is within 0.2°C of the desired value. The
differs from the certified value by 0.0001 or more units, then thermocouple is used for establishing the correct temperature
repeat the procedure given in 11.1 until a satisfactory check is level and may be removed during measurements of refractive
obtained. index. The observed reading of the thermometer at this
11.3 Measure the refractive index of API Standard temperature must be held constant to 0.02°C in the measure-
n-hexadecane and 1-methylnaphthalene at the test temperature ments to follow.
following the procedure described in Section 12. 12.2 Close the prism box and let it stand for 3 to 5 min to
ensure temperature equilibrium between the prisms and the
11.4 Construct a calibration curve for use at the chosen test
circulating bath liquid. Melt samples which are normally solid
temperature. Plot the difference between the observed refrac-
in a small container and charge as a liquid to the prism. Charge
tive index for n-hexadecane and its certified value along the
the sample from a small pipet or medicine dropper through the
ordinate against the refractive index level along the abscissa.
refractometer opening or onto the prisms open just enough to
Also plot the difference between the observed and certified
admit the sample. About 0.2 to 0.5 mL of the sample should be
refractive indices for 1-methylnaphthalene in the same manner.
allowed to flush through before completely closing the prisms.
Draw a straight line from the point representing the deviation
Samples of low volatility or high viscosity may be placed
found for n-hexadecane to zero at the certified refractive index
directly onto the prism surface by means of a stirring rod, being
of trans-decahydronaphthalene. Likewise, draw a straight line
careful not to touch the prism surface with the rod. If not
from this same zero point to the deviation found for
enough sample has been used to fill the space between the
1-methylnaphthalene.
prisms completely, or evaporation causes the field division in
11.5 If it is desired to measure the refractive index of the telescope to become uneven, clean the prisms thoroughly
samples at a temperature other than 80 or 100°C, obtain before employing a new portion of the sample.
calibration data by repeating 11.1-11.4 at this desired tempera- 12.3 Set the light source to pass rays into the illuminating
ture. Determine the refractive indices for the API Standard prism. Move the telescope by means of the adjustment screw
compounds, n-hexadecane, trans-decahydronaphthalene, and until the field division is visible in the telescope.
1-methylnaphthalene at the desired temperature by plotting the 12.4 Adjust the angle of incidence until the field consists of
certified refractive indices at 20, 25, 30, 80, and 100°C against a light and a dark portion separated by a sharp boundary, which
temperature and drawing a smooth curve between the points. may be brought into focus by sliding the telescope eyepiece. In
11.6 Precautions—In using pure liquids for calibration or the case of colloidal or suspended matter in the sample, the
checking of calibration of an Abbé-type refractometer, the boundary line may appear diffused or hazy, even though the
following precautions should be observed: telescope is perfectly focused. Filtration of the sample will
11.6.1 Before inserting the hydrocarbon calibrating liquids, sometimes correct this condition. Water in the sample may also
the prisms should be flushed with solvents and cleaned as give this hazy effect.
described in 8.2. It is advisable to preheat the solvent before 12.5 Turn the adjustment screw so that the field division
use to minimize thermal shock to the prism. This should be passes through the intersection of the crossed lines in the
followed by several such flushings with the test liquid and telescope. With the exception of extremely volatile samples, an
wiping with lens paper. After such cleaning, a reading with the interval of 2 to 3 min should be allowed before taking readings
test liquid should be taken as described in Section 11. This to permit the sample to come to the same temperature as the
should be followed by another flushing with the test liquid refractometer. In setting the edge of the field on the cross hairs,
before taking another reading of the test liquid in the prescribed at least two determinations should be obtained that agree
manner. The prisms cannot be considered free from contami- within 0.00005 to 0.0001 for precision work. The final reading
nating substances until two such determinations on the test is best obtained by approaching this setting successively from
liquid agree within the limits given in 11.6.2. both light and dark sides of the field. Read the scale through the
microscope provided. Focus by sliding the eyepiece in or out.
11.6.2 In setting the edge of the field on the cross hairs,
Measure and record the refractive index using at least two
readings should be taken in pairs, approaching the alidade
separate loadings of sample.
setting from one direction only as recommended by the
manufacturer. Several such sets will probably be necessary NOTE 6—For more reliable results with a sample that shows a diffused
before satisfactory agreement is obtained. Satisfactory agree- or hazy boundary line even after filtration, there are two possible
ment is 0.00005 to 0.0001. remedies: (1) back window reflection if the refractometer is so equipped,
or (2) dilution with a suitable solvent.
11.6.3 For results of highest accuracy, the calibration with (1) Back window reflection also permits measurements of samples too
hydrocarbons of known properties should be made immedi- dark for normal operation. The sample is charged in the normal manner.
ately before the determination on the sample. Remove the cover plate on the back of the prism housing and position the

3
 D 1747 – 99 (2004)e1
light source so that it shines directly into the opening. Bring the boundary 14.1.1 Repeatability—The difference between successive
line into view. The fields will be reversed and considerably reduced in test results obtained by the same operator with the same
contrast. Read the refractive index as described above. Care should be
apparatus under constant operating conditions on identical test
exercised during the measurement since the sharp boundary line is faint
and difficult to distinguish. material, would in the long run, in the normal and correct
(2) The dilution procedure is generally unsatisfactory and should only operation of the test method, exceed 0.00007 units of refractive
be used if it is impossible to obtain consistent readings in any other way. index only in one case in twenty.
The sample is diluted with an equal volume of high boiling solvent whose
14.1.2 Reproducibility—The difference between two single
density and refractive index are known and an appropriate correction
applied to the results. Highly aromatic or olefinic samples in the gas oil and independent results, obtained by different operators work-
range can be measured by this procedure. The possibility of volume ing in different laboratories on identical test material, would in
change on mixing should be considered. A check on the density of the the long run, in the normal and correct operation of the test
mixture will show if this occurs. method, exceed 0.0006 units of refractive index only in one
13. Calculation and Reporting case in twenty.
13.1 Correct the observed refractive index by the amount NOTE 7—The precision for this test method was not obtained in
shown in the calibration curve. Report the value of refractive accordance with RR:D02-1007.
index as:
14.2 The bias for this test method has not been determined.
nDt 5 . . . Subcommittee D02.04.0D plans to cooperatively test modern
refractometers and determine the bias.
14. Precision and Bias
14.1 The precision of the test method as obtained by 15. Keywords
statistical examination of interlaboratory test results is as
follows: 15.1 oils; purity; refractive index; refractometer; wax

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