An American National Standard

Designation: D 6550 – 00

Standard Test Method for

Determination of Olefin Content of Gasolines by
Supercritical-Fluid Chromatography 1
This standard is issued under the fixed designation D 6550; 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.

1. Scope D 6293 Test Method for Oxygenates and Paraffin, Olefin,

1.1 This test method covers the determination of the total Naphthene, Aromatic (O-PONA) Hydrocarbon Types in
amount of olefins in blended motor gasolines and gasoline Low-Olefin Spark Ignition Engine Fuels by Gas Chroma-
blending stocks by supercritical-fluid chromatography (SFC). tography
Results are expressed in terms of mass % olefins. The D 6296 Test Method for Total Olefins in Spark-ignition
application range is from 1 to 25 mass % total olefins. Engine Fuels by Multi-dimensional Gas Chromatography
1.2 This test method can be used for analysis of commercial D 6299 Practice for Applying Statistical Quality Assurance
gasolines, including those containing varying levels of oxygen- Techniques to Evaluate Analytical Measurement System
ates, such as methyl tert/butyl ether (MTBE), diisopropyl ether Performance
(DIPE), methyl tert/amyl ether (TAME), and ethanol, without 3. Terminology
interference.
3.1 Definitions of Terms Specific to This Standard:
NOTE 1—This test method has not been designed for the determination 3.1.1 critical pressure, n—the pressure needed to condense
of the total amounts of saturates, aromatics, and oxygenates.
a gas to a liquid at the critical temperature.
1.3 The values stated in SI units are to be regarded as 3.1.2 critical temperature, n—the highest temperature at
standard. The values given in parentheses are for information which a gaseous fluid can be condensed to a liquid by means
only. of compression.
1.4 This standard does not purport to address all of the 3.1.3 supercritical fluid, n—a fluid maintained above its
safety concerns, if any, associated with its use. It is the critical temperature and critical pressure.
responsibility of the user of this standard to establish appro- 3.1.4 supercritical-fluid chromatography (SFC), n—a type
priate safety and health practices and determine the applica- of chromatography that employs a supercritical fluid as the
bility of regulatory limitations prior to use. mobile phase.
2. Referenced Documents 4. Summary of Test Method
2.1 ASTM Standards: 2 4.1 A small aliquot of the fuel sample is injected onto a set
D 1319 Test Method for Hydrocarbon Types in Liquid of two chromatographic columns connected in series and
Petroleum Products by Fluorescent-Indicator Adsorption transported using supercritical carbon dioxide (CO2) as the
D 4052 Test Method for Density and Relative Density of mobile phase. The first column is packed with high-surface-
Liquids by Digital Density Meter area silica particles. The second column contains either high-
D 5186 Test Method for Determination of the Aromatic surface-area silica particles loaded with silver ions or strong-
Content and Polynuclear Aromatic Content of Diesel Fuels cation-exchange material loaded with silver ions.
and Aviation Turbine Fuels by Supercritical Fluid Chro- 4.2 Two switching valves are used to direct the different
matography classes of components through the chromatographic system to
the detector. In a forward-flow mode, saturates (normal and
1
branched alkanes, cyclic alkanes) pass through both columns to
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
the detector, while the olefins are trapped on the silver-loaded
D02.04.0C on Liquid Phase Chromatography. column and the aromatics and oxygenates are retained on the
Current edition approved April 10, 2000. Published June 2000. silica column. Aromatic compounds and oxygenates are sub-
2
For referenced ASTM standards, visit the ASTM website, [Link], or sequently eluted from the silica column to the detector in a
contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on back-flush mode. Finally, the olefins are back-flushed from the
the ASTM website. silver-loaded column to the detector.

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

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 D 6550 – 00
TABLE 1 Typical Columns
Silica Column Silver-loaded Column
vendor Merck vendor Hypersil, Phenomenex, Selerity
Packing material Lichrospher SI 60 Packing material Hypersil SCX, Selectosil SCX, Ag+ form
Particle size, µm 5 particle size, µm 5
Length, mm 250 length, mm 100 or 50
Internal diameter, mm 4.6 internal diameter, mm 4.6

4.3 A flame-ionization detector (FID) is used for quantita- [Link] A UV detector with a very small dead volume can be
tion. Calibration is based on the area of the chromatographic inserted between the column and the FID and operated in
signal for olefins, relative to standard reference materials, series.
which contain a known mass % of total olefins as corrected for [Link] A post-column splitting device, consisting of a
density. T-junction with an appropriate flow restrictor to the FID, can be
inserted between the column and the UV detector. Using the
5. Significance and Use T-junction, the two detectors can be operated in parallel. The
5.1 Gasoline-range olefinic hydrocarbons have been dem- combination of restrictors (before the FID and after the UV
onstrated to contribute to photochemical reactions in the detector) shall allow the pump and detector to perform as
atmosphere, which result in the formation of photochemical specified.
smog in susceptible urban areas. 6.1.3 Sample-inlet System—A liquid-sample injection
5.2 The California Air Resources Board (CARB) has speci- valve3 is required, capable of introducing (sub-)microlitre
fied a maximum allowable limit of total olefins in motor volume with a precision better than 0.5 %. A 1-µL injection
gasoline. This necessitates an appropriate analytical test volume was found to be adequate in combination with 4.6-mm
method for determination of total olefins to be used both by inside diameter columns. Corresponding injection volumes are
regulators and producers. 200 and 50 nL for columns with inside diameters of 2 and 1
5.3 This test method compares favorably with Test Method mm, respectively. The sample inlet system shall be installed
D 1319 (FIA) for the determination of total olefins in motor and operated in a manner such that the chromatographic
gasolines. It does not require any sample preparation, has a separation is not negatively affected.
comparatively short analysis time of about 10 min, and is 6.1.4 Columns—Two columns of equal inside diameter are
readily automated. Alternative methods for determination of required:
olefins in gasoline include Test Methods D 6293 and D 6296. [Link] A high-surface-area-silica column, capable of sepa-
rating alkanes and olefins from aromatics as specified in
6. Apparatus Section 8. Typically, one or several 250-mm long columns are
used. These columns are packed with particles having an
6.1 Supercritical-fluid Chromatograph (SFC)—Any SFC
average diameter of 5 µm or less, 600-nm (60-Å) pores, and a
instrumentation can be used that has the following character-
surface area of $350 m2/g.
istics and meets the performance requirements specified in
Section 8. NOTE 3—Columns suitable for Test Method D 5186 are also suitable
for the present method. A typical example is shown in Table 1.
NOTE 2—The SFC instruments suitable for Test Method D 5186 are
suitable for this test method, if equipped with two switching valves, as [Link] A silver-loaded-silica column or a cation-exchange
described under 6.1.7. column in the silver form. Cation-exchange columns are
6.1.1 Pump—The SFC pump shall be able to operate at the claimed4 to yield more stable columns. Typically, one 50 or
required pressures (typically up to about 30 MPa) and deliver 100-mm long column packed with particles with an average
a sufficiently stable flow to meet the requirements of retention- diameter of 5 µm is used for the analysis.
time precision (better than 0.3 %) and detection background NOTE 4—Some columns that have been used successfully are shown in
(see Section 8). The characteristics of the pump will largely Table 1.
determine the optimum column diameter. The use of 4.6-mm 6.1.5 Column-temperature Control—The chromatograph
internal diameter (i.d.) columns requires a pump capacity of at shall be capable of column temperature control to within 0.5°C
least 1 mL/min of liquid CO2. Columns with an inside diameter or less.
of 2 and 1 mm require minimum pump capacities of 200 and 6.1.6 Computor or Electronic Integrator—Means shall be
50 µL/min, respectively. provided for the determination of accumulated peak areas. This
6.1.2 Detectors—A FID is required for quantitation. A flow can be done by means of a computer or electronic integrator.
restrictor shall be installed immediately before the FID. This The computer or integrator shall have the capability of correct-
restrictor serves to maintain the required pressure in the ing for baseline shifts during the run.
column, while allowing the pump and detector to perform as
specified. A (diode-array or variable wavelength) UV detector 3
Sample valves with loop volumes down to 50 nL are commercially available
for establishing optimum switching times (see Sections 8 and
from Valco (Houston, TX).
9) is optional. Such a detector can be incorporated in two 4
Anderson, P. E., Demirbueker, M., and Blomberg, L. G., Journal of Chroma-
different manners. tography, 596, 1991, pp. 301-311.

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 D 6550 – 00

FIG. 1 Configuration of Switching Valves (Shown in Position A)

6.1.7 Switching Valves—Two six-way switching valves are 7.2 Air—Zero-grade (hydrocarbon-free) air is used as the
configured in accordance with the scheme shown in Fig. 1. FID oxidant. (Warning—Air is usually supplied as a com-
This configuration allows four different valve positions, de- pressed gas under high pressure, and it supports combustion.)
fined as follows: 7.3 Calibration Solution—A mixture of hydrocarbons with
[Link] Position A—Silica column (forward-flush mode) a known mass % of olefins of the type and concentration found
and silver-loaded column (forward-flush mode) connected in in typical gasolines. This olefin mixture can be diluted by
series. This position is used (a) to inject the sample on the two weight with olefin-free components, such as alkylate, toluene,
columns, (b) to elute the saturates, (c) to trap the olefins on the xylenes, and oxygenates, such as MTBE, as appropriate to
silver-loaded column, and (d) to retain the aromatics and approximate the composition of the fuels being tested.
oxygenates on the silica column. 7.4 Carbon Dioxide (CO 2 )—Supercritical-fluid-
[Link] Position B—Silica column (backflush mode) con- chromatographic grade, 99.99 % minimum purity, supplied
nected in-line; silver-loaded column not in flow path. This pressurized in a cylinder with a dip tube for removal of liquid
position is used to elute the aromatics and polar compounds. CO2. (Warning—Liquid at high pressure. Release of pressure
[Link] Position C—Silica column not in flow path; silver- results in production of extremely cold, solid CO2 and gas,
loaded column (backflush mode) connected in-line. This posi- which can dilute available atmospheric oxygen.)
tion is used to elute the olefins. 7.5 Hydrogen—Hydrogen of high quality (hydrocarbon-
[Link] Position D—Silica column (forward-flush mode) free) is used as the fuel for the FID. (Warning—Hydrogen is
connected in-line; silver-loaded column not in flow path. This usually supplied under high pressure and is extremely flam-
position is used to optimize the separation. Also, this position mable.)
allows Test Method D 5186 to be performed without changing 7.6 Loading-time Mixture—A mixture of a typical alkane
the system. and an olefin, which can be used to determine the loading time
(see [Link] (a) and [Link] (b)) while protecting the silver-
7. Reagents and Materials loaded column from exposure to aromatic compounds.
7.1 Purity of Reagents—Reagent grade chemicals shall be 7.7 Performance Mixture—A mixture of a typical alkane, a
used in all tests. Unless otherwise indicated, it is intended that mono-aromatic (usually toluene), and a typical mono-olefin
all reagents conform to the specifications of the Committee on can be used to fine-tune this test method and to check its
Analytical Reagents of the American Chemical Society where performance. A mixture of n-heptane, toluene, and 3-methyl-
such specifications are available.5 Other grades may be used, 2-pentene has been successfully used for this purpose.
provided it is first ascertained that the reagent is of sufficiently 7.8 Quality Control Sample—A motor gasoline containing
high purity to permit its use without lessening the accuracy of olefins to be used to establish and monitor the precision of the
the determination. analytical measurement system.
8. Preparation of Apparatus
5
Reagent Chemicals, American Chemical Society Specifications, American 8.1 Install the SFC instrumentation in accordance with the
Chemical Society, Washington, DC. For suggestions on the testing of reagents not manufacturer’s instructions. System operating conditions will
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
depend on the column used and optimization of performance.
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, The conditions listed in Table 1 have been used successfully. If
MD. the performance characteristics in terms of retention and

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 D 6550 – 00
resolution, specified in 8.2, are not achieved, the temperature, any peaks (SBaseline) to within 0.1 % of the height of the
pressure, or mobile-phase flow rate can be modified to achieve aromatics peak (hAromatics), that is,
compliance. A silica column of low activity can be reactivated SEnd # SBaseline 1 hAromatics / 1000 (2)
by solvent rinsing, using accepted liquid-chromatographic
activation strategies. [Link] Silver-loaded Column—This column is operated
exclusively as an olefin trap. Its stability and chromatographic
8.2 System Performance:
efficiency are not critical as long as the following two require-
8.2.1 System Optimization—The operation of the SFC sys- ments are met. The column shall allow a quantitative separa-
tem shall be optimized in order to achieve the required tion between the saturates and the olefins and the quantitative
separation on the silica column. This process is different if an release of all olefins under appropriate conditions. The perfor-
optional UV detector is available. mance of the silver-loaded column can be verified indepen-
[Link] When the optional UV detector is installed, the dently of that of the silica column by switching the valves to
separation between the three different classes of compounds the appropriate position (see [Link]).
can be monitored directly. Saturates show no UV absorption.
Olefins show significant absorption at wavelengths up to about NOTE 5—It is recommended that aromatic solutes should not be
220 nm but no absorption at 250 nm or higher. Aromatics show introduced on the silver-loaded column. This can be achieved by using a
loading-time mixture, which does not contain aromatics, or by using the
considerable absorption at low wavelengths, extended to a
silica column to trap the latter.
wavelength of 250 nm and higher. The onset of the elution of
the olefin fraction (following the saturates fraction) can be (a) When using a quality control sample for optimization, as
monitored at 220 nm. The elution of the aromatic fraction can will typically be the case when a UV detector is installed, no
be monitored at 250 nm. In this case, the performance mixture olefins shall elute from the silver-loaded column in the
(see 7.6) can be used to optimize the separation of the olefins forward-flush mode in a time, tL, defined as:
and aromatics. tL 5 tSAT 1 33 ySAT (3)
[Link] Without a UV detector being installed, individual
pure components and the performance mixture (see 7.6) can be where:
used to optimize the system. tSAT = time for the saturated-peak apex, s, and
ySAT = peak width at half height of the saturates peak, s.
8.2.2 Column Requirements:
(b) When using a performance mixture for optimization, as
[Link] Silica Column—The critical requirement for the
will typically be the case when using only an FID detector, no
silica column is its ability to achieve a quantitative separation
olefins shall elute from the silver-loaded column in the
between the olefins and aromatics. The performance of this
forward-flush mode in a time, tL, defined as:
column can be verified independently of that of the silver-
loaded column by switching the valves to the appropriate tL 5 tS 1 5 3 yS (4)
position (see [Link]). where:
[Link].1 When using a UV detector, the requirement is tS = retention time for the saturates reference compound, s,
baseline resolution between the olefin and aromatic signals. and
The resulting switching time (see Section 9) shall be chosen to yS = peak width at half height for the saturates reference
occur just before the onset of the aromatics signal. compound, s.
[Link].2 When using only an FID, the resolution (RAO) (c) All olefins shall be released from the silver-loaded
between the olefinic compound and the aromatic compound in column in the backflush mode within a time, tBF, that is less
the performance mixture shall be at least three when measured than five times the total time during which the olefins are
as follows: loaded onto the column in the forward-flush mode (tFF), that is,
2 3 ~ tA 2 t O ! tBF # 5 3 tFF (5)
RAO 5 (1)
1.699 3 ~yA 1 yO!
The total time tFF is the sum of the loading time (tL) and a
where: cleaning time (tC):
tA = retention time for the aromatic reference compound, tFF 5 tL 1 tC (6)
s,
tO = retention time for the olefinic reference compound, s, During the time tC, any non-olefinic (saturates or cyclic)
yA = peak width at half height for the aromatic reference compounds that have remained in the olefin trap are eluted in
compound, s, and the forward-flush mode. The absence of an FID signal at the
yO = peak width at half height for the olefinic reference end of the time tC confirms proper separation between saturated
compound, s. (including cyclic) and olefinic compounds. The elution of the
[Link] All aromatic compounds, as well as oxygenates and olefins can be observed using either a UV-absorbance detector
other polar molecules, are eluted from the silica column in the set at 220 nm or an FID. Complete elution is thought to have
backflush mode during a time, tAR, which shall be less than five occurred if the detector value (SEnd) has returned to the
times the loading time, tL. The elution of the aromatics and baseline value observed before the elution of the saturates or
polars can be observed using an FID. Complete elution is olefins (SBaseline), or both, to within 0.1 % of the height of the
thought to have occurred if the detector value (SEnd) has olefins peak (hOlefins), that is,
returned to the baseline value observed before the elution of SEnd # SBaseline 1 hOlefins / 1000 (7)

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 D 6550 – 00
NOTE 6—It may be necessary to change the operating conditions in TABLE 2 Typical SFC Conditions
order to meet the requirement of Eq 5. Increasing the mobile-phase Parameter Value
density or the column temperature may facilitate the elution of the olefins.
Temperature, °C 75
However, the best precision can be achieved if the conditions are kept Column-outlet pressure, MPa 22.3A
constant. CO2 flow rate, mL/min 2.5B
Injection volume, µL 1
8.2.3 Retention-time Precision: FID temperature, °C 350
[Link] Repeatability—The repeatability of the retention Air, mL/min 300
Hydrogen, mL/min 50
times has a direct influence on the precision of the total olefin Air make-up, mL/min 15
content determined because column switching is performed on Analysis time, min 5-20
a time basis (see Section 9). Retention times obtained for A
As regulated at the column-outlet.
performance mixtures and standard gasolines on a given B
Liquid CO2 under pump conditions.
instrument and column set shall be repeatable within 0.5 %
(relative) over a period of several days.
[Link] If both columns are positioned in the flow path, use
NOTE 7—It has been observed that the first analysis after an idle period the loading-time mixture (see 7.5) to protect the silver-loaded
often results in somewhat different retention times than those previously column.
determined for the test method.
9.2.2 Determine the time period, tAR, required to back-flush
[Link] Reproducibility—The reproducibility of the reten- all aromatic and polar compounds from the silica column after
tion times from column to column and from instrument to the loading-time period, tL, using a quality control sample.
instrument is not critical, provided that the column perfor- Columns are initially connected in series (see [Link]). Valves
mance requirements (see 8.2) are met. are switched at the end of time period, tL, such that only the
8.2.4 Calibration Curve: silica column is in the flow path (back-flush mode; see [Link]).
[Link] A calibration curve shall be generated by blending at Measurement of tAR can then be made while protecting the
least four different calibration solutions of known olefin silver-loaded column from aromatics.
content. Olefin-free gasoline blending components and aromat- 9.2.3 Determine the time period, tC, required to clean all
ics shall be used to dilute a known olefin mixture to produce saturated and cyclic compounds from the silver-loaded column
standards. A mixture of alkylate, toluene, xylenes, and appro- in the forward-flush mode, using a quality control sample.
priate oxygenates (MTBE, and so forth) shall be used to Columns are initially connected in series (see [Link]). Valves
prepare calibration solutions. These calibration solutions shall are switched at time, tL, such that only the silica column is in
be of known density (see 9.1) the flow path (see [Link]). Valves are then switched at the end
[Link] These calibration standards shall be blended to cover of time period, tAR, (total time = tL + tAR). The silica and
the entire range of olefin content for which the test method will silver-loaded columns are connected in series (see [Link]),
be used. The calibration curve is a plot of the observed peak allowing the elution of the saturated and cyclic compounds.
area for the entire olefin signal against the known mass The time period, tC, shall be short enough to avoid the onset of
percentage of olefins in the calibration standards. Analysis of a the elution of olefins from the silver-loaded column.
blank shall also be used to confirm no olefin contamination in 9.2.4 Determine the time period, tBF, required to elute all
the hydrocarbon mixture used to prepare the standards. olefins from the silver-loaded column in the backflush mode.
Columns are initially connected in series (see [Link]). Valves
[Link] The intercept of the calibration curve (extrapolated
are switched at the end of time period, tL, such that only the
peak area to zero olefin concentration) shall not be statistically
silica column is in the flow path (see [Link]). Valves are then
different from zero.
switched at the end of time period, tAR, such that the two
NOTE 8—If the intercept of the calibration curve is not zero, then one columns are again connected in series (see [Link]). Valves are
of the materials (alkylate, reformate, and so forth) used to blend the switched at the end of time period, tC, (total time tL+ tAR + tC)
standards may not be olefin free. These shall be analyzed individually to such that only silver-loaded column is in the flow path in the
determine which is contaminated.
backflush mode (see [Link]), allowing the elution of the
olefins. The resulting switching table, with typical values
9. Procedure
corresponding to the conditions listed in Table 1 and Table 2,
9.1 Determination of Density of Samples and Standards— is shown as Table 3.
Determine density of samples and standards using Test Method 9.3 Application of this Test Method:
D 4052 or equivalent. 9.3.1 Calibration Curve—Record the calibration curve, as
9.2 Switching Times: described in 8.2.4.
9.2.1 Establish the loading time period, tL, between injec- 9.3.2 Analyzing Samples—Inject undiluted aliquots of all
tion (t = 0) and the onset of the aromatic peak, as described in gasoline samples. An example chromatogram is shown as Fig.
[Link]. 2 (see Fig. 3 for the details of Fig. 2).
[Link] Only the silica column need be in the flow path to
the detector (forward-flush mode; see [Link]) for this step. 10. Calculation
This will protect the silver-loaded column from aromatics (see 10.1 Determine the total area of the olefins peak. Determine
[Link]) when using a quality control sample to determine the the total concentration of olefins directly from the calibration
loading time period. curve. An example of a calibration curve is shown in Fig. 4.

5
 D 6550 – 00
TABLE 3 Switching Table with Typical Time Values attained, corrective action shall be taken, verified by successful
NOTE 1—Other times can be used if they produce equivalent or better analysis of the quality control sample.
results.
12. Report
Time Valve Typical Time, min Action
Period Position 12.1 Report the total olefin concentration to the nearest 0.1
tL A initial - 1.4 loading sample onto col-
mass % for values exceeding 1 mass %.
umns; eluting saturates
13. Precision and Bias 6
tAR B 1.4 – 4 eluting aromatics 13.1 The precision of this test method as determined by the
tC A 4 - 4.5 eluting remaining saturates statistical examination of interlaboratory test results is as
from olefin trap follows.
13.1.1 Repeatability—The difference between successive
tBF C 4.5 – 10 eluting olefins
results obtained by the same operator with the same apparatus
under constant operating conditions on identical test materials
would, in the long run, in the normal and correct operation of
10.2 When the density of the standards used for calibration the test method, exceed the values in Table 4 only in one case
is different from the samples being analyzed, a density correc- in twenty.
tion shall be applied. This can be accomplished using the Repeatability = 0.11 X0.75
following calculation: where X is between 1 and 25 mass % olefin
Mcor 5 Mcal [~rstd!/ ~rsam!# (8) 13.1.2 Reproducibility—The difference between two single
and independent results obtained by different operators work-
where: ing in different laboratories on identical test materials would, in
Mcor = corrected mass % olefin, the long run, in the correct operation of the test method, exceed
Mcal = mass % olefins as interpolated from calibration the values in Table 4 only in one case in twenty:
curve, Reproducibility = 0.47 X0.75
rstd = density of the standard solution used to make the where X is between 1 and 25 mass % olefin
calibration curve, and 13.2 Bias—No information can be presented on the bias of
rsam = density of gasoline sample. this test method because no material having an accepted
reference value is available.
11. Quality Control
11.1 Prior to the analysis of any samples in a given 24-h 14. Keywords
period, the laboratory shall analyze at least one quality control 14.1 motor gasolines; olefins; supercritical-fluid chromatog-
sample, using the procedure defined in 9.2. Results from the raphy; unsaturated hydrocarbons
analysis of the quality control sample shall be in statistical
control in accordance with Practice D 6299, or other equivalent 6
Supporting data have been filed at ASTM Headquarters. Request
practice. Otherwise, if agreement with the expected value is not RR:D02–1478.

6
 D 6550 – 00

NOTE 1—See Fig. 3 for detailed display of the olefin region.

FIG. 2 Example Chromatogram of Conventional Gasoline

FIG. 3 Detailed Display of Olefin Region of Chromatogram Shown in Fig. 2

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 D 6550 – 00

FIG. 4 Typical Calibration Curve

TABLE 4 Precision Estimate—Total Olefins

Total Olefin, Repeatability, Reproducibility,
mass % mass % mass %
1 0.1 0.5
3 0.3 1.1
5 0.4 1.6
10 0.6 2.6
15 0.8 3.6
20 1.0 4.4
25 1.2 5.3

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