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.

Designation: D1218 − 12 (Reapproved 2016)

Standard Test Method for

Refractive Index and Refractive Dispersion of Hydrocarbon
Liquids1
This standard is issued under the fixed designation D1218; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope and/or mercury containing products into your state or country

1.1 This test method covers the measurement of refractive may be prohibited by law.
index, accurate to four decimal places or better, of transparent 1.6 This standard does not purport to address all of the
and light-colored hydrocarbons in the range of 1.3300 to safety concerns, if any, associated with its use. It is the
1.5000 at temperatures from 20 °C to 30 °C by manual responsibility of the user of this standard to establish appro-
(optical-mechanical) or automatic (digital) procedure. priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.2 The manual (optical-mechanical) procedure also covers
the measurement of refractive dispersion accurate to the fourth
2. Referenced Documents
decimal place or better.
NOTE 1—The test method may be suitable for measuring the refractive 2.1 ASTM Standards:2
indices of liquids above 1.5000 and at temperatures both below 20 °C and D1193 Specification for Reagent Water
above 30 °C; however, the test method precision may not apply. Verifi- D1500 Test Method for ASTM Color of Petroleum Products
cation of the accuracy of such measurements will depend upon the
availability of reliable, certified reference standards that demonstrate the (ASTM Color Scale)
performance of the instrument used under the particular measuring D6299 Practice for Applying Statistical Quality Assurance
conditions. and Control Charting Techniques to Evaluate Analytical
1.3 The test method may not be applicable to liquids that are Measurement System Performance
strongly colored, or that have bubble points so near the test D6300 Practice for Determination of Precision and Bias
temperature that a reading cannot be obtained before substan- Data for Use in Test Methods for Petroleum Products and
tial weathering takes place. Liquid color should be limited to Lubricants
No. 4 ASTM Color or lighter, as determined by Test Method E1 Specification for ASTM Liquid-in-Glass Thermometers
D1500. 2.2 ASTM Adjuncts:
1.4 The values stated in SI units are to be regarded as Determination of Precision and Bias Data for Use in Test
standard. No other units of measurement are included in this Methods for Petroleum Products and Lubricants, Version
standard. 4.0.653
1.5 WARNING—Mercury has been designated by many 3. Terminology
regulatory agencies as a hazardous material that can cause
central nervous system, kidney and liver damage. Mercury, or 3.1 Definitions:
its vapor, may be hazardous to health and corrosive to 3.1.1 refractive dispersion, n—the difference between the
materials. Caution should be taken when handling mercury and refractive indices of a substance for light of two different
mercury containing products. See the applicable product Ma- wavelengths, both indices being measured at the same tem-
terial Safety Data Sheet (MSDS) for details and EPA’s perature.
website—http://www.epa.gov/mercury/faq.htm—for addi- 3.1.1.1 Discussion—For convenience in calculations, the
tional information. Users should be aware that selling mercury value of the difference thus obtained is usually multiplied by
10 000.

1
This test method is under the jurisdiction of ASTM Committee D02 on
2
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Subcommittee D02.04.0D on Physical and Chemical Methods. contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Current edition approved Oct. 1, 2016. Published November 2016. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1952. Last previous edition approved in 2012 as D1218 – 12. DOI: the ASTM website.
3
10.1520/D1218-12R16. Out of print. No longer available from ASTM International Headquarters.

*A Summary of Changes section appears at the end of this standard

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3.1.2 refractive index, n—the ratio of the velocity of light 6.4 Light Sources—The following type of light source can
(of specified wavelength) in air, to its velocity in the substance be used in conjunction with an optical-mechanical (Abbe type)
under examination. refractometer:
3.1.2.1 Discussion—It may also be defined as the sine of the 6.4.1 Sodium Arc Lamp, NaD line at 589 nm.
angle of incidence divided by the sine of the angle of 6.4.2 Mercury Arc Lamp, Hgc line at 546 nm or Hgg line at
refraction, as light passes from air into the substance. This is 436 nm.
the relative index of refraction. If absolute refractive index 6.4.3 Cadmium Arc Lamp, CdC’ line at 644 nm.
(that is, referred to vacuum) is desired, this value should be
6.4.4 Mercury-Cadmium Arc Lamp.
multiplied by the factor 1.00027, the absolute refractive index
of air. The numerical value of refractive index of liquids varies 6.4.5 Helium Discharge Lamp.
inversely with both wavelength and temperature. NOTE 3—Measurement of refractive dispersion requires more than one
type of light source.
4. Summary of Test Method
6.5 Light Filters—Arc lamps can emit a number of spectral
4.1 The refractive index is measured using a high-resolution lines that result in multiple-borderlines observed in the refrac-
refractometer of an optical-mechanical or automatic digital tometer. Filters can be used to eliminate unwanted lines
type with the prism temperature accurately controlled. The (borderlines). Depending upon instrument design, the manu-
instrument principle is based on the critical angle concept. facturer will recommend and supply a suitable filter or adapt a
commercially-available filter (for example, interference filter)
5. Significance and Use to suit the application.
5.1 Refractive index and refractive dispersion are funda-
mental physical properties, which can be used in conjunction 7. Reagents and Materials
with other properties to characterize pure hydrocarbons and 7.1 n-Pentane, 95 mol % Minimum Purity, for cleaning the
their mixtures. prism faces. (Warning—Flammable. Harmful if inhaled. Va-
pors may cause flash fire.)
PROCEDURE A—MANUAL (OPTICAL- NOTE 4—Low boiling hydrocarbon fractions with boiling range 50 °C
MECHANICAL) PROCEDURE to 100 °C have also been found to be acceptable.
7.2 Toluene, HPLC Grade, for cleaning the prism faces.
6. Apparatus (Warning—Flammable. Vapor harmful.)
6.1 Refractometer, high-resolution optical-mechanical re- 7.3 1-Bromonaphthalene, 98 mol % Minimum Purity, con-
fractometer of the “Abbe” type with suitable measuring range tact liquid when calibrating with solid reference standard.
(1.3300 to 1.5000 or higher) and an accuracy/resolution of (Warning—Toxic when ingested.)
0.0001 or better refractive index.
7.4 Primary Reference Materials, for calibrating the instru-
NOTE 2—Prior to 2001, Test Method D1218 was based on a Bausch & ment.
Lomb Refractometer. However, this instrument is no longer manufactured.
Currently available manual refractometers are of the “Abbe” type (critical 7.4.1 Solid Reference Standard, with the value of refractive
angle refractometers, see X1.2.3). There is a variety of refractometers that index engraved on its upper face.
have been found to be suitable for this measurement. Some instruments 7.4.2 Distilled or Deionized Water, conforming to Type II or
offer a wider measuring range but it is important to verify the uniformity
of accuracy across the entire measuring range and to ensure suitable III of Specification D1193. At 20 °C, nD = 1.3330; at 25 °C,
calibration materials are available for this verification. nD = 1.3325; and at 30 °C, nD = 1.3319
6.2 Temperature Control Unit, either an external liquid bath 7.4.3 2,2,4-trimethylpentane, 99 mol % Minimum Purity, at
with both heating and cooling capability and pump for main- 20 °C, nD = 1.3915; at 25 °C, nD = 1.3890.
taining the indicated prism temperature within 0.1 °C, or an 7.4.4 Methylcyclohexane, 99 mol % Minimum Purity, at
internal electronic temperature control system (such as Peltier 20 °C, nD = 1.4231; at 25 °C, nD = 1.4206.
system). If an external bath is used, the thermostating liquid 7.4.5 Toluene, 99 mol % Minimum Purity, at 20 °C,
shall pass the temperature measuring device on leaving, not on n D = 1.4969; at 25 °C, n D = 1.4941. (Warning—2,2,4-
entering the prism. The temperature control unit (external or trimethylpentane, methylcylcohexane, and toluene are all flam-
internal) shall have the following control specification: mable. Their vapor can be harmful.)
Stability ±0.1 °C NOTE 5—Other pure materials may be used to calibrate the instrument
Uniformity ±0.1 °C as primary reference material, as long as they can be obtained in 99 mol %
Display Resolution 0.1 °C or better minimum purity and accurate values of their refractive indices at specific
6.3 Temperature Measuring Device, for those apparatus temperatures are available. The precision of the test method (see 15.1 and
24.1) were obtained using distilled water as the calibrant.
employing mercury in glass thermometer, ASTM Thermometer
17C having a range from 19 °C to 27 °C, and conforming to the 7.5 Secondary Reference Materials, for calibrating the
requirements of Specification E1. For apparatus using non- instrument.
mercury in glass thermometer, a platinum resistance probe, 7.5.1 Mineral Oil Calibration Standards, measured and
thermocouple, or equivalent temperature sensors are accept- certified by suppliers for specific refractive index ranges and
able. temperatures.
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8. Sampling 11.2 For optimum accuracy, use a reference material whose
8.1 A sample of at least 0.5 mL is required. The sample shall refractive index is close to the desired refractive index range
be free of suspended solids, water, or other materials that may and temperature to calibrate the instrument.
settle onto the prism surface and affect the measured reading.
12. Procedure
Water can be removed from hydrocarbons by treatment with
calcium chloride followed by filtering or centrifuging to 12.1 Ensure that the prism faces are clean and dry. Check
remove the desiccant. The possibility of changing the compo- that the prism temperature is within 0.1 °C of the desired
sition of the sample by action of the drying agent, by selective temperature.
adsorption on the filter, or by fractional evaporation, shall be 12.2 Unlock (if necessary) and open the prism assembly.
considered. (Warning—Volatile hydrocarbon samples are
12.3 Place one or two drops of the sample on the lower
flammable.)
prism face. Close the prism assembly and lock (if necessary).
Turn on the light source. Allow 3 min temperature equilibra-
9. Preparation of Apparatus
tion time.
9.1 The refractometer shall be kept scrupulously clean at all
12.4 Look through the eyepiece and observe the field
times. Dust and oil can impair the optical component of the
consisting of a light and dark portion. Follow manufacturer’s
instrument. Thoroughly clean the prism faces with toluene,
instructions to adjust the instrument so that the boundary
followed by n-pentane (see Note 4) (Warning—These mate-
between the light and dark portions of the field is as sharp as
rials are extremely flammable. Harmful if inhaled. Vapors may
possible.
cause flash fire.) using cotton swabs, fresh clean lens tissue, or
similar material, in accordance with manufacturer’s instruc- 12.5 Following manufacturer’s instructions, make any ad-
tions. Do not dry the prism faces by rubbing with dry cotton. ditional adjustment until the sharp boundary line intersects the
midpoint of the crosshairs superimposed on the field.
9.2 Adjust the thermostat bath/circulator settings or the
electronic temperature control system so that the temperature 12.6 Read the refractive index on the scale. Repeat 12.5 at
indicated by the refractometer temperature measuring device is least four times, approaching from either side of the sharp
within 0.1 °C of the desired value. Turn on the light source and boundary line, and average the scale readings.
allow the refractometer to equilibrate for 30 min. 12.7 Record and report the average refractive index value.
NOTE 6—The constancy of the prism temperature can be seriously
affected by variations in ambient conditions such as air drafts or changes 12.8 If instrument is capable of determining refractive
in room temperature. Reasonable precautions should be taken to minimize dispersion, change the light source to a light source with
these factors. different wavelength. Determine the refractive index at the
secondary wavelength following 12.4 – 12.7.
10. Calibration of Refractometer Using Solid Reference NOTE 7—When determining refractive dispersion, it is expected that the
Standard instrument would have been calibrated at both wavelengths used.
10.1 Thoroughly clean the prism faces and surfaces of the 13. Quality Control
solid reference standard (see 7.4.1). Open the prism assembly.
Apply a drop of 1-bromonaphthalene contact liquid, about 13.1 Confirm the performance of the test procedure by
1.5 mm in diameter, to the center of the polished surface of the analyzing a quality control (QC) sample, which is stable and
solid reference material. Press the reference standard against representative of the sample of interest.
the surface of the prism face with the polished end towards the 13.1.1 When quality control/quality assurance (QC/QA)
light source. protocols are established in the testing facility, these may be
used to confirm the reliability of the test result.
10.2 Follow the manufacturer’s instructions on how to 13.1.2 When there are no QC/QA protocols established in
calibrate the instrument using the solid reference standard. the testing facility, Appendix X4 can be used to provide
10.3 If the observed refractive index differs from the value guidelines in performing this function.
engraved on the solid reference standard by more than 0.0001,
adjust the refractometer’s scale reading to match the certified 14. Calculation and Report
value, following manufacturer’s instructions. 14.1 Report the average refractive index to four decimal
places and the test temperature at which the test was made, for
11. Calibration of the Refractometer Using Liquid example:
Reference Standards
n D 5 x.xxxx at 20 °C or n 589 5 x.xxxx at 20 °C (1)
11.1 Using the procedure described in Section 12, determine
the refractive index of any of the Reference Materials specified where D or the 589 signifies that the sodium D spectral line
in 7.4 or 7.5 for a specific test temperature. If the observed was used.
refractive index for the chosen reference material at a specified 14.2 If a refractive dispersion measurement was made,
test temperature differs by more than 0.0001 of the listed value, calculate the absolute value of the difference between the
make adjustment to the instrument following manufacturer’s refractive indices at the two wavelengths and multiply the
instructions so that the observed refractive index corresponds difference by 10 000. Report the calculated value and the test
to the listed value. temperature, for example:
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? ~n g ?
2 n D ! 3 104 at t 5 20 °C (2) 16.5 Light Filters—See 6.5.
where g and D signifies that the mercury g and sodium D 17. Reagents and Materials
spectral lines were used in the measurement.
17.1 See Section 7.
15. Precision and Bias
15.1 Precision—Refractive Index: 18. Sampling
15.1.1 The precision for the manual (optical-mechanical) 18.1 See Section 8.
refractive index procedure, as determined by the statistical
examination of interlaboratory test results conducted in 19964 19. Preparation of Apparatus
on eight different samples from ten laboratories, is as follows: 19.1 See Section 9. Ensure that the instrument has a solvent
15.1.2 Repeatability— The difference between successive resistant prism seal.
test results, obtained by the same operator with the same
apparatus, under constant operating conditions, and on identi- 20. Calibration of the Refractometer Using Liquid
cal test material, would, in the long run, in the normal and Reference Standards
correct operation of the test method, exceed the following
values only in one case in twenty (95 % confidence level): 20.1 Automatic digital refractometers are normally cali-
brated using liquid reference standards (see 7.4 and 7.5). They
r manual 5 0.0002 (3) may require a single, two-point, or multi-point calibration.
15.1.3 Reproducibility— The difference between two, single Follow manufacturer’s instruction in calibrating the particular
and independent results obtained by different operators work- automatic digital refractometer being used.
ing in different laboratories on identical test material would, in
the long run, in the normal and correct operation of the test 21. Procedure
method, exceed the following values only in one case in twenty 21.1 Ensure that the prism and the surrounding plate and
(95 % confidence level): dish/plate (and presser, if fitted) are thoroughly cleaned as in
R manual 5 0.0005 (4) 9.1. Ensure the prism temperature is correct and the instrument
has been properly calibrated.
15.1.4 The precision of this test method for automatic and
21.2 Introduce the test sample to the prism ensuring that the
manual refractive index was obtained in accordance with
prism is adequately covered. Do not introduce an excessive
Practice D6300 using the D02 Precision Program (D2PP)
amount because this can slow the thermal equilibration. Lower
software.3
the sample presser (if fitted).
15.2 Precision—Refractive Dispersion:
21.3 Take a succession of readings, noting values, until a
15.2.1 Repeatability = 0.00012
steady value is obtained. Record or report, or both, this value
15.2.2 Reproducibility = 0.00012
as the refractive index of the sample at the test temperature.
15.2.3 The precision for refractive dispersion was not ob-
NOTE 8—From experience using the instrument, the user will be able to
tained in accordance with Practice D6300, and was not part of judge with a safe margin the amount of time needed for a sample to
the 1996 interlaboratory study. 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.
PROCEDURE B—AUTOMATIC (DIGITAL) NOTE 9—When successive readings are drifting, the direction of drift
PROCEDURE 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
16. Apparatus warming up. This is particularly noticeable when samples are much hotter
or cooler than the prism.
16.1 Refractometer—Automatic digital refractometer with a
suitable measuring range of 1.3300 to 1.5000 or higher, 22. Quality Control
capable of displaying the measured refractive index automati-
22.1 See Section 13.
cally and digitally. The instrument shall incorporate a solvent-
resistant prism seal.
23. Report
16.2 Temperature Control Unit—See 6.2.
23.1 An automatic digital electronic refractometer shall
16.3 Temperature Measuring Device—A platinum resis- provide a direct and digital reading of refractive index. This
tance probe or equivalent. The accuracy and resolution of the can be manually recorded or, if the refractometer is equipped
temperature measuring device shall be 0.1 °C or better. with a computer interface, readings can be sent to a printer or
16.4 Light Source—Filtered white light such as that ob- to a computer.
tained using a tungsten-halogen lamp or a light emitting diode 23.2 Report the refractive index to four decimal places and
(LED), capable of providing the sodium D spectral line at the test temperature, for example:
589 nm. n D 5 x.xxxx at 20 °C or n 589 5 x.xxxx at 20 °C (5)
4
Supporting data have been filed at ASTM International Headquarters and may where D or the 589 signifies that the sodium D spectral line
be obtained by requesting Research Report RR:D02-1493. was used.

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24. Precision and Bias ing in different laboratories on identical test material would, in
24.1 Precision—Refractive Index: the long run, in the normal and correct operation of the test
24.1.1 The precision for the automatic digital refractive method, exceed the following values only in one case in twenty
index procedure, as determined by the statistical examination (95 % confidence level):
of interlaboratory test results conducted in 19964 on eight R automatic 5 0.0005 (7)
different samples from ten laboratories, is as follows:
24.1.2 Repeatability—The difference between successive 24.1.4 The precision of this test method for automatic
test results, obtained by the same operator with the same refractive index was obtained in accordance with Practice
apparatus, under constant operating conditions, and on identi- D6300 using the D02 Precision Program (D2PP) software.3
cal test material, would, in the long run, in the normal and 24.2 Relative Bias—The 1996 interlaboratory study did not
correct operation of the test method, exceed the following indicate any relative bias between automatic and manual
values only in one case in twenty (95 % confidence level): refractive index instruments.
r automatic 5 0.0002 (6)

24.1.3 Reproducibility—The difference between two, single 25. Keywords

and independent results obtained by different operators work- 25.1 refractive dispersion; refractive index; refractometer

APPENDIXES

(Nonmandatory Information)

X1. FACTORS THAT AFFECT PRECISION AND ACCURACY

X1.1 Temperature —Refractive index varies inversely and can utilize a white light source, but often these instruments are
non-linearly with temperature. The relative change in refrac- limited in accuracy because of the light source. High accuracy
tive index with temperature (temperature coefficient) is differ- Abbe refractometers require a pure spectral light source such as
ent for each liquid under test. Hydrocarbon liquids have a a sodium arc lamp (see 6.4).
higher temperature coefficient than water and aqueous solu- X1.2.4 Modern electronic digital refractometers function at
tions. For example, at 20 °C the temperature coefficient for a single wavelength, invariably that of sodium light (589 nm).
water is –9 × 10–5 units of refractive index per °C. For The refractive index at this wavelength is denoted as nD.
hydrocarbon liquids, the coefficient will typically be in the
range –3 × 10–4 to –5 × 10–4. X1.2.5 One of two types of light source tends to be used in
digital refractometers: (1) filtered white light source such as
X1.2 Wavelength (Light Source) that obtained using a tungsten-halogen lamp, or ( 2) light
X1.2.1 Refractive index also varies inversely and non- emitting diode (LED).
linearly with the wavelength of light. Refractive index should, X1.2.6 With both types of light source, the wavelength is
therefore, be measured using light of a single wavelength not a single value but is a narrow band spanning typically
(monochromatic light). Most measurements traditionally have 10 nm or more about the nominal value (589 nm). The degree
been made at the sodium D line (589.3 nm) because of the of impurity (band width) will cause a dispersion of the detected
purity and availability of a sodium source such as an arc lamp. light from the sample. Instrument software can be used to
Other light sources include mercury, cadmium, helium, and compensate for and thus minimize this error source but it will
hydrogen where filters are used with the refractometer to nevertheless be a factor in determining the limiting accuracy of
eliminate unwanted emission lines. the instrument. The dispersion error will however differ ac-
cording to the substance measured. This is why instrument
X1.2.2 The effect of wavelength on refractive index is
manufacturers may specify the instrument accuracy as typically
called dispersion. Different substances have varying degrees of
or better than in order to cover a broad application scope.
refractive dispersion (sometimes called dispersive power).
NOTE X1.1—Sodium actually emits a doublet of lines at 589.1 nm and
X1.2.3 Optical-mechanical refractometers (often called 589.6 nm. However, for practical purposes, because of the proximity of
Abbe refractometers or critical angle refractometers) can be the lines, it is regarded as a single wavelength source and the average
used with a variety of spectral light sources. Some instruments value of 589.3 nm is often cited.

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X2. INSTRUMENT CALIBRATION

X2.1 A refractometer must be calibrated using one or more switched on and the liquid bath circulation is started, a period
reliable calibration standards. The optical system in a refrac- of thermal adjustment is required to allow the internal
tometer is subject to microscopic movement as materials environment, and particularly the optical system, to adjust to
expand and contract with fluctuating ambient thermal condi- the new condition. Calibration should not take place until the
tions. This effect leads to calibration drift, which must be instrument is in a steady-state. Experience will demonstrate
periodically corrected to ensure measurement reliability. that this may be typically up to an hour. Similarly, if the
circulating liquid temperature is changed, a new calibration
X2.2 Calibration materials are available as two types: solids sequence will be required. In circumstances where the instru-
(test plates) and liquids. Solid plates are often preferred for ment is used continuously and in a constant thermal condition,
their stability (shelf life), but have the disadvantage of limited the need for recalibration should be minimal.
accuracy in use because of the errors associated with the
placing of the plate on the refractometer prism. Typically, a X2.5 For each calibration point, a calibration standard is
plate may not allow an accuracy better than 60.0001 units of required. Any calibration fluid could be used. However, it is
refractive index. Test plates are particularly difficult to apply to best practice to select fluids with a refractive index close to the
sapphire prisms of the type typically used in digital electronic intended measuring range or, where a pair or group of
refractometers. This is because the micro-roughness of sap- standards is needed, select liquids that adequately span the
phire is greater than that of softer (optically flatter) glasses used working range.
in optical (Abbe) refractometers. Invariably, liquid reference
standards will be preferred and will be recommended by X2.6 Whether an electronic digital instrument or an optical-
instrument manufacturers for this reason. mechanical instrument is being used, the laboratory needs to
X2.3 An optical-mechanical instrument may require cali- adopt a strict protocol for calibration frequency and procedure.
bration at only one point on the scale. Automatic digital This will entail regular checks on measurement accuracy
refractometers may require a single (zero), two-point, or (verification) using reliable standards. The calibration should
multi-point calibration. For each calibration a suitable calibra- only be reset when measured values are outside of the stated
tion standard should be used. tolerance. The protocol should also include procedures that
govern the control of calibration materials: storage (shelf-life),
X2.4 The frequency of calibration will depend upon a contamination-prevention and staff competence (approved us-
number of factors. When an electronic instrument is first ers).

X3. REFLECTED VERSUS TRANSMITTED LIGHT

X3.1 Critical angle refractometers can function by using optical-mechanical (Abbe) instruments because of the low light
light transmission through the sample (usually a thin film intensity and poor contrast.
sandwiched between two prisms) or by light reflection. A light
reflection mechanism has the advantage that effects of absorp- X3.2 Digital electronic refractometers usually work with a
tion (highly colored samples) are minimized. A disadvantage of reflected light mechanism.
reflectance is the difficulty of observing the borderline in

X4. GUIDELINES FOR QUALITY CONTROL

X4.1 The performance of the instrument or the test proce- X4.3 Prior to monitoring the measurement process, the
dure should be confirmed by analyzing a quality control (QC) average value and control limits of the QC sample need to be
sample. established (see Practice D6299 and ASTM MNL 75). When a
new QC sample material is required, control limits for the new
X4.2 It is recommended that the QC sample be representa- material should be established before the old QC sample is
tive of the material routinely analyzed. However, pure materi- exhausted.
als 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 5
ASTM MNL7, “Manual on Presentation of Data Control Chart Analysis,” 6th
storage conditions. Edition, available from ASTM International Headquarters.

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X4.4 The QC results should be recorded, and analyzed by stability of the testing process, the length of time required to do
control charts or other statistically equivalent techniques to the test, and customer requirements. The QC testing frequency
ascertain the statistical control status of the total testing process should be increased if a large number of samples are routinely
(see Practice D6299 and ASTM MNL 75). Any out of control analyzed. However, when it is demonstrated that the test
data should trigger an investigation of root cause(s). The method is under statistical control, the QC testing frequency
results of such investigation may, but not necessarily, result in may be reduced. The QC sample precision should be checked
instrument recalibration. against the ASTM method precision to ensure quality of
results.
X4.5 In the absence of explicit requirements given in the
test method, the frequency of QC testing is dependent on the X4.6 Consult Practice D6299 and ASTM MNL 75 for
criticality of the quality being measured, the demonstrated further guidance on QC and control charting techniques.

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