Índice de Refração - D-1218

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Designation: D 1218 02 (Reapproved 2007)

An American National Standard

Standard Test Method for

Refractive Index and Refractive Dispersion of Hydrocarbon


Liquids1
This standard is issued under the fixed designation D 1218; 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.

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

4. Summary of Test Method


4.1 The refractive index is measured using a high-resolution
refractometer of an optical-mechanical or automatic digital

This test method is under the jurisdiction of ASTM Committee D02 on


Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.04.0D on Physical and Chemical Methods.
Current edition approved Nov. 1, 2007. Published January 2008. Originally
approved in 1952. Last previous edition approved in 2002 as D 121802.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
the ASTM website.

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.

type with the prism temperature accurately controlled. The


instrument principle is based on the critical angle concept.
5. Significance and Use
5.1 Refractive index and refractive dispersion are fundamental physical properties, which can be used in conjunction
with other properties to characterize pure hydrocarbons and
their mixtures.

7. Reagents and Materials


7.1 n-Pentane, 95 mol % Minimum Purity, for cleaning the
prism faces. (WarningFlammable. Harmful if inhaled. Vapors may cause flash fire.)
NOTE 4Low boiling hydrocarbon fractions with boiling range 50 to
100C have also been found to be acceptable.

PROCEDURE AMANUAL (OPTICALMECHANICAL) PROCEDURE

7.2 Toluene, HPLC Grade, for cleaning the prism faces.


(WarningFlammable. Vapor harmful.)
7.3 1-Bromonaphthalene, 98 mol % Minimum Purity, contact liquid when calibrating with solid reference standard.
(WarningToxic when ingested.)
7.4 Primary Reference Materials, for calibrating the instrument.
7.4.1 Solid Reference Standard, with the value of refractive
index engraved on its upper face.
7.4.2 Distilled or Deionized Water, conforming to Type II or
III of Specification D 1193. At 20C, nD = 1.3330; at 25C,
nD = 1.3325; and at 30C, nD = 1.3319
7.4.3 2,2,4-trimethylpentane, 99 mol % Minimum Purity, at
20C, nD = 1.3915; at 25C, nD = 1.3890.
7.4.4 Methylcyclohexane, 99 mol % Minimum Purity, at
20C, nD = 1.4231; at 25C, nD = 1.4206.
7.4.5 Toluene, 99 mol % Minimum Purity, at 20C,
n D = 1.4969; at 25C, n D = 1.4941. (Warning2,2,4trimethylpentane, methylcylcohexane, and toluene are all flammable. Their vapor can be harmful.)

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.

6.2 Temperature Control Unit, either an external liquid bath


with both heating and cooling capability and pump for maintaining the indicated prism temperature within 0.1C, or an
internal electronic temperature control system (such as Peltier
system). If an external bath is used, the thermostating liquid
shall pass the temperature measuring device on leaving, not on
entering the prism. The temperature control unit (external or
internal) shall have the following control specification:
Stability
Uniformity
Display Resolution

NOTE 5Other pure materials may be used to calibrate the instrument


as primary reference material, as long as they can be obtained in 99 mol %
minimum purity and accurate values of their refractive indices at specific
temperatures are available. The precision of the test method (see 15.1 and
24.1) were obtained using distilled water as the calibrant.

6 0.1C
6 0.1C
0.1C or better

6.3 Temperature Measuring Device, for those apparatus


employing mercury in glass thermometer, ASTM Thermometer
17C having a range from 19 to 27C, and conforming to the
requirements of Specification E 1. For apparatus using nonmercury in glass thermometer, a platinum resistance probe,
thermocouple, or equivalent temperature sensors are acceptable.
6.4 Light SourcesThe following type of light source can
be used in conjunction with an optical-mechanical (Abbe type)
refractometer:
6.4.1 Sodium Arc Lamp, NaD line at 589 nm.
6.4.2 Mercury Arc Lamp, Hgc line at 546 nm or Hgg line at
436 nm.
6.4.3 Cadmium Arc Lamp, CdC line at 644 nm.
6.4.4 Mercury-Cadmium Arc Lamp.
6.4.5 Helium Discharge Lamp.

7.5 Secondary Reference Materials, for calibrating the


instrument.
7.5.1 Mineral Oil Calibration Standards, measured and
certified by suppliers for specific refractive index ranges and
temperatures.

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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.)

NOTE 3Measurement of refractive dispersion requires more than one


type of light source.

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,

6.5 Light FiltersArc lamps can emit a number of spectral


lines that result in multiple-borderlines observed in the refractometer. Filters can be used to eliminate unwanted lines
(borderlines). Depending upon instrument design, the manuCopyright ASTM International
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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.

NOTE 7When determining refractive dispersion, it is expected that the


instrument would have been calibrated at both wavelengths used.

13. Quality Control


13.1 Confirm the performance of the test procedure by
analyzing a quality control (QC) sample, which is stable and
representative of the sample of interest.
13.1.1 When quality control/quality assurance (QC/QA)
protocols are established in the testing facility, these may be
used to confirm the reliability of the test result.
13.1.2 When there are no QC/QA protocols established in
the testing facility, Appendix X4 can be used to provide
guidelines in performing this function.

10. Calibration of Refractometer Using Solid Reference


Standard
10.1 Thoroughly clean the prism faces and surfaces of the
solid reference standard (see 7.4.1). Open the prism assembly.
Apply a drop of 1-bromonaphthalene contact liquid, about 1.5
mm in diameter, to the center of the polished surface of the
solid reference material. Press the reference standard against
the surface of the prism face with the polished end towards the
light source.
10.2 Follow the manufacturers instructions on how to
calibrate the instrument using the solid reference standard.
10.3 If the observed refractive index differs from the value
engraved on the solid reference standard by more than 0.0001,
adjust the refractometers scale reading to match the certified
value, following manufacturers instructions.

14. Calculation and Report


14.1 Report the average refractive index to four decimal
places and the test temperature at which the test was made, for
example:
nD 5 x.xxxx at 20C or n589 5 x.xxxx at 20C

11. Calibration of the Refractometer Using Liquid


Reference Standards
11.1 Using the procedure described in Section 12, determine
the refractive index of any of the Reference Materials specified
in 7.4 or 7.5 for a specific test temperature. If the observed
refractive index for the chosen reference material at a specified
test temperature differs by more than 0.0001 of the listed value,
make adjustment to the instrument following manufacturers
instructions so that the observed refractive index corresponds
to the listed value.
11.2 For optimum accuracy, use a reference material whose
refractive index is close to the desired refractive index range
and temperature to calibrate the instrument.

where D or the 589 signifies that the sodium D spectral line


was used.
14.2 If a refractive dispersion measurement was made,
calculate the absolute value of the difference between the
refractive indices at the two wavelengths and multiply the
difference by 10 000. Report the calculated value and the test
temperature, for example:
? ~ng 2 nD! ? 3 104 at t 5 20C

(2)

where g and D signifies that the mercury g and sodium D


spectral lines were used in the measurement.
15. Precision and Bias
15.1 PrecisionRefractive Index:
15.1.1 The precision for the manual (optical-mechanical)
refractive index procedure, as determined by the statistical
examination of interlaboratory test results conducted in 19964
on eight different samples from ten laboratories, is as follows:
15.1.2 RepeatabilityThe difference between successive
test results, obtained by the same operator with the same
apparatus, under constant operating conditions, and on identical test material, would, in the long run, in the normal and

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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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.

correct operation of the test method, exceed the following


values only in one case in twenty (95 % confidence level):
rmanual 5 0.0002

(3)

15.1.3 ReproducibilityThe difference between two, single


and independent results obtained by different operators working in different laboratories on identical test material would, in
the long run, in the normal and correct operation of the test
method, exceed the following values only in one case in twenty
(95 % confidence level):
Rmanual 5 0.0005

(4)

15.1.4 The precision of this test method for automatic and


manual refractive index was obtained in accordance with
Practice D 6300 using the D02 Precision Program (D2PP)
software.3
15.2 PrecisionRefractive Dispersion:
15.2.1 Repeatability = 0.00012
15.2.2 Reproducibility = 0.00012
15.2.3 The precision for refractive dispersion was not obtained in accordance with Practice D 6300, and was not part of
the 1996 interlaboratory study.

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.

PROCEDURE BAUTOMATIC (DIGITAL)


PROCEDURE

22. Quality Control


22.1 See Section 13.

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

where D or the 589 signifies that the sodium D spectral line


was used.
24. Precision and Bias
24.1 PrecisionRefractive Index:
24.1.1 The precision for the automatic digital refractive
index procedure, as determined by the statistical examination
of interlaboratory test results conducted in 19964 on eight
different samples from ten laboratories, is as follows:
24.1.2 RepeatabilityThe difference between successive
test results, obtained by the same operator with the same
apparatus, under constant operating conditions, and on identical test material, would, in the long run, in the normal and
correct operation of the test method, exceed the following
values only in one case in twenty (95 % confidence level):

17. Reagents and Materials


17.1 See Section 7.
18. Sampling
18.1 See Section 8.
19. Preparation of Apparatus
19.1 See Section 9. Ensure that the instrument has a solvent
resistant prism seal.
20. Calibration of the Refractometer Using Liquid
Reference Standards
20.1 Automatic digital refractometers are normally calibrated using liquid reference standards (see 7.4 and 7.5). They
may require a single, two-point, or multi-point calibration.
Follow manufacturers instruction in calibrating the particular
automatic digital refractometer being used.

rautomatic 5 0.0002

(6)

24.1.3 ReproducibilityThe difference between two, single


and independent results obtained by different operators working in different laboratories on identical test material would, in
the long run, in the normal and correct operation of the test
method, exceed the following values only in one case in twenty
(95 % confidence level):

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D 1218 02 (2007)
Rautomatic 5 0.0005

(7)

25. Keywords

24.1.4 The precision of this test method for automatic


refractive index was obtained in accordance with Practice
D 6300 using the D02 Precision Program (D2PP) software.3
24.2 Relative BiasThe 1996 interlaboratory study did not
indicate any relative bias between automatic and manual
refractive index instruments.

25.1 refractive dispersion; refractive index; refractometer

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.

X1.1 TemperatureRefractive index varies inversely and


non-linearly with temperature. The relative change in refractive index with temperature (temperature coefficient) is different for each liquid under test. Hydrocarbon liquids have a
higher temperature coefficient than water and aqueous solutions. For example, at 20C the temperature coefficient for
water is -9 3 10-5 units of refractive index per C. For
hydrocarbon liquids, the coefficient will typically be in the
range -3 3 10-4 to -5 3 10-4.
X1.2 Wavelength (Light Source)
X1.2.1 Refractive index also varies inversely and nonlinearly with the wavelength of light. Refractive index should,
therefore, be measured using light of a single wavelength
(monochromatic light). Most measurements traditionally have
been made at the sodium D line (589.3 nm) because of the
purity and availability of a sodium source such as an arc lamp.
Other light sources include mercury, cadmium, helium, and
hydrogen where filters are used with the refractometer to
eliminate unwanted emission lines.
X1.2.2 The effect of wavelength on refractive index is
called dispersion. Different substances have varying degrees of
refractive dispersion (sometimes called dispersive power).
X1.2.3 Optical-mechanical refractometers (often called
Abbe refractometers or critical angle refractometers) can be
used with a variety of spectral light sources. Some instruments

NOTE X1.1Sodium actually emits a doublet of lines at 589.1 and


589.6 nm. However, for practical purposes, because of the proximity of
the lines, it is regarded as a single wavelength source and the average
value of 589.3 nm is often cited.

X2. INSTRUMENT CALIBRATION

X2.1 A refractometer must be calibrated using one or more


reliable calibration standards. The optical system in a refractometer is subject to microscopic movement as materials
expand and contract with fluctuating ambient thermal conditions. This effect leads to calibration drift, which must be
periodically corrected to ensure measurement reliability.

refractive index. Test plates are particularly difficult to apply to


sapphire prisms of the type typically used in digital electronic
refractometers. This is because the micro-roughness of sapphire is greater than that of softer (optically flatter) glasses used
in optical (Abbe) refractometers. Invariably, liquid reference
standards will be preferred and will be recommended by
instrument manufacturers for this reason.

X2.2 Calibration materials are available as two types:


solids (test plates) and liquids. Solid plates are often preferred
for their stability (shelf life), but have the disadvantage of
limited accuracy in use because of the errors associated with
the placing of the plate on the refractometer prism. Typically,
a plate may not allow an accuracy better than 60.0001 units of

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.

best practice to select fluids with a refractive index close to the


intended measuring range or, where a pair or group of
standards is needed, select liquids that adequately span the
working range.
X2.6 Whether an electronic digital instrument or an opticalmechanical instrument is being used, the laboratory needs to
adopt a strict protocol for calibration frequency and procedure.
This will entail regular checks on measurement accuracy
(verification) using reliable standards. The calibration should
only be reset when measured values are outside of the stated
tolerance. The protocol should also include procedures that
govern the control of calibration materials: storage (shelf-life),
contamination-prevention and staff competence (approved
users).

X2.5 For each calibration point, a calibration standard is


required. Any calibration fluid could be used. However, it is

X3. REFLECTED VERSUS TRANSMITTED LIGHT

X3.1 Critical angle refractometers can function by using


light transmission through the sample (usually a thin film
sandwiched between two prisms) or by light reflection. A light
reflection mechanism has the advantage that effects of absorption (highly colored samples) are minimized. A disadvantage of
reflectance is the difficulty of observing the borderline in

optical-mechanical (Abbe) instruments because of the low light


intensity and poor contrast.
X3.2 Digital electronic refractometers usually work with a
reflected light mechanism.

X4. GUIDELINES FOR QUALITY CONTROL

X4.4 The QC results should be recorded, and analyzed by


control charts or other statistically equivalent techniques to
ascertain the statistical control status of the total testing process
(see Practice D 6299 and ASTM MNL 75). Any out of control
data should trigger an investigation of root cause(s). The
results of such investigation may, but not necessarily, result in
instrument recalibration.

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.

X4.5 In the absence of explicit requirements given in the


test method, the frequency of QC testing is dependent on the
criticality of the quality being measured, the demonstrated
stability of the testing process, the length of time required to do
the test, and customer requirements. The QC testing frequency
should be increased if a large number of samples are routinely
analyzed. However, when it is demonstrated that the test
method is under statistical control, the QC testing frequency
may be reduced. The QC sample precision should be checked
against the ASTM method precision to ensure quality of
results.

X4.3 Prior to monitoring the measurement process, the


average value and control limits of the QC sample need to be
established (see Practice D 6299 and ASTM MNL 75). When a
new QC sample material is required, control limits for the new
material should be established before the old QC sample is
exhausted.

X4.6 Consult Practice D 6299 and ASTM MNL 75 for


further guidance on QC and control charting techniques.

ASTM MNL7, Manual on Presentation of Data Control Chart Analysis, 6th


Edition, available from ASTM International Headquarters.

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D 1218 02 (2007)

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