ASTM F3417-20

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: F3417 − 20
Standard Test Method for
Gas Chromatography Analysis of Petroleum Waxes Used in
Equestrian Synthetic Surfaces
This standard is issued under the fixed designation F3417; 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.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 The slack waxes typically used in equestrian surfaces
D4307 Practice for Preparation of Liquid Blends for Use as
comprise a blend of different waxes and oils, with various
Analytical Standards
hydrocarbons, chain lengths and structures.
D4626 Practice for Calculation of Gas Chromatographic
1.2 The blend of wax and oil determines the mechanical
Response Factors
propertiesofthesurfacematerial,aswellastheresponseofthe
D5442 TestMethodforAnalysisofPetroleumWaxesbyGas
wax to temperature. The combination of lower and higher
Chromatography
carbon weight materials, oil content, and hydrocarbon struc-
E260 Practice for Packed Column Gas Chromatography
tures also controls how the wax will endure over time. As the
E355 Practice for Gas Chromatography Terms and Relation-
wax ages, it is expected that lower density components will be
ships
lost at a higher rate than higher density materials.
3. Terminology
1.3 The gas chromatography (GC) test is used to determine
3.1 Definitions of Terms Specific to This Standard:
the carbon number distribution in extracted wax samples for
3.1.1 carbon number, n—number corresponding to the num-
both normal and abnormal hydrocarbons (linear vs. non-linear
ber of carbon atoms in a hydrocarbon.
carbon chains). This procedure is outlined in Test Method
D5442. GC testing utilizes a chromatograph with a flame 3.1.2 cool on-column injection, n—sample introduction
ionization detector and column. technique in gas chromatography where the sample is injected
inside the front portion of a partition column at a temperature
1.4 The values stated in SI units are to be regarded as
at or below the boiling point of the most volatile component in
standard. No other units of measurement are included in this
the sample.
standard.
3.1.3 low volume connector, n—metal or glass union de-
1.5 This standard does not purport to address all of the
signed to connect two lengths of capillary tubing. Usually
safety concerns, if any, associated with its use. It is the
designed so that the tubing ends are joined with a minimum of
responsibility of the user of this standard to establish appro-
either dead volume or overlap between them.
priate safety, health, and environmental practices and deter-
3.1.4 non(normal paraffın) hydrocarbon (NON), n—all
mine the applicability of regulatory limitations prior to use.
other hydrocarbon types excluding those hydrocarbons with
1.6 This international standard was developed in accor-
carbonatomsinalinearchain.Includesaromatics,naphthenes,
dance with internationally recognized principles on standard-
and branched hydrocarbon types.
ization established in the Decision on Principles for the
3.1.5 normal paraffın, n—saturated hydrocarbon that has
Development of International Standards, Guides and Recom-
solely linearly bonded carbon atoms without branching or
mendations issued by the World Trade Organization Technical
hydrocarbon rings.
Barriers to Trade (TBT) Committee.
3.1.6 wall coated open tube (WCOT), n—term used to
specify capillary columns in which the stationary phase is
This test method is under the jurisdiction of ASTM Committee F08 on Sports
Equipment, Playing Surfaces, and Facilities and is the direct responsibility of For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Subcommittee F08.28 on Equestrian Surfaces. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Jan. 1, 2020. Published February 2020. DOI: 10.1520/
Standards volume information, refer to the standard’s Document Summary page on
F3417-20. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F3417 − 20
TABLE 1 Typical Operating Conditions
coated on the interior surface of the glass or fused silica tube.
Stationary phase may be cross-linked or bonded after coating. Column length (m) 25 30 15
Column inside diameter 0.32 0.53 0.25
(mm)
4. Summary of Test Method
Stationary phase DB-1 RTX-1 DB-5
methyl silicone methyl silicone 5 % phenyl
4.1 Wax samples are thoroughly stirred, and 0.2 g of the
methyl silicone
wax is dissolved in 2.0 ml of cyclohexane.The solution is then
Film thickness (µm) 0.25 0.25 0.25
sonicated for 15 min and transferred by pipette into a GC vial Carrier gas Helium Helium Helium
Carrier flow (mL/min) 1.56 5.0 2.3
and sealed. A solvent blank GC vial of cyclohexane is also
Linear velocity (cm/s) 33 35 60
prepared. The wax-cyclohexane mixture is introduced into a
Column initial 80 80 80
temperature (°C)
gas chromatographic high-temperature column that separates
Program rate (°C/min) 10 8 5
the hydrocarbon components by increasing carbon number.
Final temperature (°C) 380 340 350
The column temperature is increased at a reproducible rate
Injection technique cool on-column cool on-column cool on-column
Detector temperature 380 400 375
until the sample is completely eluted from the column. The
(°C)
temperature of the column must be able to reach at least
Sample size (µL) 1.0 1.0 1.0
400.0°C.
4.2 The eluted components are detected by a flame ioniza-
tion detector (FID) and recorded on a strip chart or computer
provided the system meets the specification for linearity of
system. The individual carbon numbers are identified by
response in 10.6. For cool on-column injection, syringes with
comparing the retention times obtained from a qualitative
0.15 to 0.25-mm outside diameter needles have been used
standard with the retention times of the wax sample. The
successfully for columns 0.25 mm inside diameter or larger
percent of each hydrocarbon number through C is calculated
and standard 0.47 mm outside diameter syringe needles have
via internal standard calculations after applying response
been used for columns 0.53 mm inside diameter or greater.
factors.
6.2.1 Care must be taken that the sample size chosen does
4.3 For samples with final boiling points greater than
not allow any peaks to exceed the linear range of the detector
538.0°C complete elution of all components may not be or overload the capacity of the column.
achieved under the specified conditions. For this reason, the
6.3 Column(s)—Any column used must meet the chromato-
C material is determined by summing the concentrations of
45+
graphic resolution specification in 10.5. WCOT columns with
each individual carbon number through C and subtracting
25 to 30 m lengths and a stationary phase coating of methyl
this total from 100.00 mass %.
siloxane or 5 % phenyl methyl siloxane have been successfully
used. Cross-linked or bonded stationary phases are preferred.
5. Significance and Use
6.4 Recorder—Arecordingpotentiometerorequivalentwith
5.1 The determination of the carbon number distribution of
a full-scale deflection of 5 mV or less for measuring the
petroleum-based waxes used in synthetic equestrian tracks is
detector signal versus time. Full scale response time should be
useful for characterizing the overall molecular composition to
2 s or less. Sensitivity and stability should be sufficient enough
aid in binder selection and replenishment. The test data is also
to generate greater than 2 mm recorder deflection for a
very useful for comparing carbon number distributions be-
hydrocarbon injection of 0.05 mass % under the analysis
tween different binders and monitoring an existing track binder
conditions employed.
as it ages over time.The oil extracted from the wax can also be
6.5 Integrator or Computer—Means must be provided for
analyzed by this method. Track surface maintenance decisions
integrating the detector signal and summing the peak areas
can be aided by the results of this test.
between specific time intervals. Peak areas can be measured by
computerorelectronicintegration.Thecomputer,integrator,or
6. Apparatus
gas chromatograph must have the capability of subtracting the
6.1 Chromatograph—Any gas chromatographic instrument
area corresponding to the baseline (blank) from the sample
thatcanaccommodateaWCOTcolumn,equippedwithaflame
area, and have the ability to draw the baselines used for peak
ionization detector, and that can be operated at the conditions
area integration.
given in Table 1 may be employed. The chromatograph should
be equipped with a cool on-column inlet (or equivalent) for
7. Reagents and Materials
introducing appropriate quantities of sample without fraction-
7.1 Carrier Gas—Carrier gas appropriate for the FID.
ation. In addition, the gas chromatograph must be capable of
Hydrogen and helium have been used successfully. The mini-
generating a chromatogram where the retention times of an
mum purity of the carrier gas used should be 99.95 mol %.
individual peak have retention time repeatability within 0.1
(Warning—Hydrogen and helium are compressed gases under
min. Refer to Practices E260 and E355 for general information
high pressure. Hydrogen is an extremely flammable gas.)
on gas chromatography.
7.2 n-hexadecane—Hydrocarbon to be added to samples as
6.2 Sample Introduction System—Any system capable of
an internal standard. Minimum purity of 98 % is required.
introducing a representative sample onto the front portion of a
WCOTcolumn may be employed. Cool on-column injection is 7.3 Standards for Calibration and Identification—Standard
preferred, however other injection techniques can be used samples of normal paraffins covering the carbon number range
F3417 − 20
(through C ) of the sample are needed for establishing the 9.2 Aluminum foil usually contains a thin film of oil from
retention times of the individual paraffins and for calibration processing. This oil must be removed by rinsing the foil with
for quantitative measurements. Hydrocarbons used for stan- solvent such as hexane or mineral spirits, prior to use.
dards must be greater than 95 % purity.
10. Preparation of Apparatus
7.4 Solvent—A liquid (99 % pure) suitable for preparing a
quantitative mixture of hydrocarbons and for dissolving petro-
10.1 Column Conditioning—Capillary columns with
leum wax. Cyclohexane has been used successfully.
bonded (or cross-linked) stationary phases do not normally
(Warning—Solvents are flammable and harmful if inhaled.)
need to be conditioned; however, it is good chromatographic
practice to briefly condition a new column as described below.
7.5 Linearity Standard—Prepare a weighted mixture of
10.1.1 Install the column in the chromatographic oven and
n-paraffins covering the range between n-C to n-C and
16 44
connectonecolumnendtothesampleinletsystem.Turnonthe
dissolve the mixture in cyclohexane. Use approximately equal
source of carrier gas and set the flow controller (or pressure
amounts of each of the paraffins and a balance capable of
regulator) to the flow rate to be used in the analysis. Increase
determining mass to within1%ofthe mass of each compound
thecolumntemperaturetothemaximumvaluetobeusedinthe
added. It is not necessary to include every n-paraffin in this
analysis and maintain this temperature for 30 min. Cool the
mixture so long as the sample contains n-C , n-C , and at
16 44
column temperature to room temperature and connect the
least one of every fourth n-paraffin. It will be necessary to
remaining column end to the detector. Care must be taken that
prepare the standard sample in cyclohexane, so that the normal
the column terminates as close as possible to the tip of the FID
paraffins are completely dissolved in the solvent. Solutions of
jet. The temperature of the column between the column oven
0.01 mass % n-paraffin have been used successfully. This
and the detector jet must be maintained above the maximum
sample must be capped tightly, to prevent solvent loss which
column temperature.
willchangetheconcentrationofparaffinsinthestandardblend.
10.2 Operating Conditions—Set the chromatographic oper-
NOTE 1—Refer to Practice D4307 for details of how to prepare
hydrocarbon mixtures.
ating conditions (see Table 1) and allow the system to achieve
all temperature set points. The recorder, computer or integrat-
7.6 Internal Standard Solution—Prepare a dilute solution of
ing device should be connected so that a plot of the detector
internal standard in cyclohexane in two steps as follows:
signal versus time can
...