ASTM D7455-08
(Practice)Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
SIGNIFICANCE AND USE
Crude oil, petroleum, petroleum products, additives, and lubricants are routinely analyzed for their elemental content such as chlorine, nitrogen, phosphorus, sulfur, and various metals using a variety of analytical techniques. Some of these test methods require little to no sample preparation; some others require only simple dilutions; while others require elaborate sample decomposition before the product is analyzed for its elemental content.
Fairly often it can be shown that the round robin results by a co-operator are all biased with respect to those from other laboratories. Presumably, the failure to follow good laboratory practices and instructions in the test methods can be a causal factor of such errors. A further consequence is an unnecessarily large reproducibility estimate or the data being dropped from the study as an outlier.
Uniform practice for sample preparation is beneficial in standardizing the procedures and obtaining consistent results across the laboratories.
SCOPE
1.1 This practice covers different means by which petroleum product and lubricant samples may be prepared before the measurement of their elemental content using different analytical techniques.
1.2 This practice includes only the basic steps for generally encountered sample types. Anything out of the ordinary may require special procedures. See individual test methods for instructions to handle such situations.
1.3 This practice is not a substitute for a thorough understanding of the actual test method to be used, caveats the test method contains, and additional sample preparation that may be required.
1.4 The user should not expand the scope of the test methods to materials or concentrations outside the scope of the test methods being used without thoroughly understanding the implications of such deviations.
1.5 This practice may also be applicable to sample preparation of non-petroleum based bio-fuels for elemental analysis. Currently, work is ongoing in ASTM Subcommittee D02.03; as information becomes available, it will be added to this standard.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D7455 − 08
StandardPractice for
Sample Preparation of Petroleum and Lubricant Products
for Elemental Analysis
This standard is issued under the fixed designation D7455; 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 This practice covers different means by which petro-
D86 Test Method for Distillation of Petroleum Products at
leumproductandlubricantsamplesmaybepreparedbeforethe
Atmospheric Pressure
measurement of their elemental content using different analyti-
D129 Test Method for Sulfur in Petroleum Products (Gen-
cal techniques.
eral High Pressure Decomposition Device Method)
1.2 This practice includes only the basic steps for generally
D482 Test Method for Ash from Petroleum Products
encountered sample types. Anything out of the ordinary may
D808 Test Method for Chlorine in New and Used Petroleum
require special procedures. See individual test methods for
Products (High Pressure Decomposition Device Method)
instructions to handle such situations.
D874 Test Method for Sulfated Ash from Lubricating Oils
1.3 This practice is not a substitute for a thorough under-
and Additives
standing of the actual test method to be used, caveats the test
D1018 Test Method for Hydrogen In Petroleum Fractions
method contains, and additional sample preparation that may
D1091 Test Methods for Phosphorus in Lubricating Oils and
be required.
Additives
D1266 Test Method for Sulfur in Petroleum Products (Lamp
1.4 The user should not expand the scope of the test
Method)
methods to materials or concentrations outside the scope of the
D1318 Test Method for Sodium in Residual Fuel Oil (Flame
test methods being used without thoroughly understanding the
Photometric Method)
implications of such deviations.
D1548 Test Method for Vanadium in Heavy Fuel Oil
1.5 This practice may also be applicable to sample prepa- 3
(Withdrawn 1997)
ration of non-petroleum based bio-fuels for elemental analysis.
D1552 Test Method for Sulfur in Petroleum Products (High-
Currently,workisongoinginASTMSubcommitteeD02.03;as
Temperature Method)
information becomes available, it will be added to this stan-
D2622 Test Method for Sulfur in Petroleum Products by
dard.
Wavelength Dispersive X-ray Fluorescence Spectrometry
D2784 Test Method for Sulfur in Liquefied Petroleum Gases
1.6 The values stated in SI units are to be regarded as
(Oxy-Hydrogen Burner or Lamp)
standard. No other units of measurement are included in this
D3120 Test Method for Trace Quantities of Sulfur in Light
standard.
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
1.7 This standard does not purport to address all of the
lometry
safety concerns, if any, associated with its use. It is the
D3228 Test Method for Total Nitrogen in Lubricating Oils
responsibility of the user of this standard to establish appro-
and Fuel Oils by Modified Kjeldahl Method
priate safety and health practices and determine the applica-
D3230 Test Method for Salts in Crude Oil (Electrometric
bility of regulatory limitations prior to use.
Method)
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on Standards volume information, refer to the standard’s Document Summary page on
Elemental Analysis. the ASTM website.
Current edition approved May 1, 2008. Published June 2008. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D7455-08. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7455 − 08
D3231 Test Method for Phosphorus in Gasoline and Determination of Selected Elements in Base Oils by
D3237 TestMethodforLeadinGasolinebyAtomicAbsorp- Inductively Coupled Plasma Atomic Emission Spectrom-
tion Spectroscopy etry (ICP-AES)
D3246 Test Method for Sulfur in Petroleum Gas by Oxida-
D5291 Test Methods for Instrumental Determination of
tive Microcoulometry
Carbon, Hydrogen, and Nitrogen in Petroleum Products
D3340 Test Method for Lithium and Sodium in Lubricating
and Lubricants
Greases by Flame Photometer
D5384 Test Methods for Chlorine in Used Petroleum Prod-
D3341 Test Method for Lead in Gasoline—Iodine Mono-
ucts (Field Test Kit Method)
chloride Method
D5453 Test Method for Determination of Total Sulfur in
D3348 Test Method for Rapid Field Test for Trace Lead in
Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel
Unleaded Gasoline (Colorimetric Method)
Engine Fuel, and Engine Oil by Ultraviolet Fluorescence
D3605 Test Method for Trace Metals in Gas Turbine Fuels
D5600 Test Method for Trace Metals in Petroleum Coke by
by Atomic Absorption and Flame Emission Spectroscopy
Inductively Coupled Plasma Atomic Emission Spectrom-
D3701 Test Method for Hydrogen Content of Aviation
etry (ICP-AES)
Turbine Fuels by Low Resolution Nuclear Magnetic
D5622 Test Methods for Determination of Total Oxygen in
Resonance Spectrometry
Gasoline and Methanol Fuels by Reductive Pyrolysis
D3831 Test Method for Manganese in Gasoline By Atomic
D5708 Test Methods for Determination of Nickel,
Absorption Spectroscopy
Vanadium, and Iron in Crude Oils and Residual Fuels by
D4045 Test Method for Sulfur in Petroleum Products by
Inductively Coupled Plasma (ICP) Atomic Emission
Hydrogenolysis and Rateometric Colorimetry
Spectrometry
D4047 Test Method for Phosphorus in Lubricating Oils and
D5762 Test Method for Nitrogen in Petroleum and Petro-
Additives by Quinoline Phosphomolybdate Method
leum Products by Boat-Inlet Chemiluminescence
D4057 Practice for Manual Sampling of Petroleum and
D5863 Test Methods for Determination of Nickel,
Petroleum Products
Vanadium, Iron, and Sodium in Crude Oils and Residual
D4177 Practice for Automatic Sampling of Petroleum and
Fuels by Flame Atomic Absorption Spectrometry
Petroleum Products
D6334 Test Method for Sulfur in Gasoline by Wavelength
D4294 Test Method for Sulfur in Petroleum and Petroleum
Dispersive X-Ray Fluorescence
Products by Energy Dispersive X-ray Fluorescence Spec-
D6443 TestMethodforDeterminationofCalcium,Chlorine,
trometry
Copper, Magnesium, Phosphorus, Sulfur, and Zinc in
D4628 Test Method for Analysis of Barium, Calcium,
Unused Lubricating Oils and Additives by Wavelength
Magnesium, and Zinc in Unused Lubricating Oils by
Dispersive X-ray Fluorescence Spectrometry (Mathemati-
Atomic Absorption Spectrometry
cal Correction Procedure)
D4629 Test Method for Trace Nitrogen in Liquid Petroleum
D6445 Test Method for Sulfur in Gasoline by Energy-
HydrocarbonsbySyringe/InletOxidativeCombustionand
Dispersive X-ray Fluorescence Spectrometry (Withdrawn
Chemiluminescence Detection
2009)
D4808 Test Methods for Hydrogen Content of Light
D6470 Test Method for Salt in Crude Oils (Potentiometric
Distillates, Middle Distillates, Gas Oils, and Residua by
Method)
Low-Resolution Nuclear Magnetic Resonance Spectros-
D6481 Test Method for Determination of Phosphorus,
copy
Sulfur, Calcium, and Zinc in Lubrication Oils by Energy
D4927 Test Methods for Elemental Analysis of Lubricant
Dispersive X-ray Fluorescence Spectroscopy
and Additive Components—Barium, Calcium,
D6595 Test Method for Determination of Wear Metals and
Phosphorus, Sulfur, and Zinc by Wavelength-Dispersive
ContaminantsinUsedLubricatingOilsorUsedHydraulic
X-Ray Fluorescence Spectroscopy
Fluids by Rotating Disc ElectrodeAtomic Emission Spec-
D4929 Test Methods for Determination of Organic Chloride
trometry
Content in Crude Oil
D6667 Test Method for Determination of Total Volatile
D4951 Test Method for Determination ofAdditive Elements
Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum
in Lubricating Oils by Inductively Coupled Plasma
Gases by Ultraviolet Fluorescence
Atomic Emission Spectrometry
D6728 Test Method for Determination of Contaminants in
D5056 Test Method for Trace Metals in Petroleum Coke by
Gas Turbine and Diesel Engine Fuel by Rotating Disc
Atomic Absorption
Electrode Atomic Emission Spectrometry
D5059 Test Methods for Lead in Gasoline by X-Ray Spec-
D6732 Test Method for Determination of Copper in Jet
troscopy
Fuels by Graphite Furnace Atomic Absorption Spectrom-
D5184 Test Methods for Determination of Aluminum and
etry
Silicon in Fuel Oils by Ashing, Fusion, Inductively
Coupled Plasma Atomic Emission Spectrometry, and D6920 Test Method forTotal Sulfur in Naphthas, Distillates,
Atomic Absorption Spectrometry Reformulated Gasolines, Diesels, Biodiesels, and Motor
Fuels by Oxidative Combustion and Electrochemical De-
D5185 TestMethodforDeterminationofAdditiveElements,
Wear Metals, and Contaminants in Used Lubricating Oils tection
D7455 − 08
D7039 Test Method for Sulfur in Gasoline and Diesel Fuel 4.2 Fairly often it can be shown that the round robin results
by MonochromaticWavelength Dispersive X-ray Fluores- by a co-operator are all biased with respect to those from other
cence Spectrometry laboratories. Presumably, the failure to follow good laboratory
D7040 Test Method for Determination of Low Levels of practices and instructions in the test methods can be a causal
factorofsucherrors.Afurtherconsequenceisanunnecessarily
Phosphorus in ILSAC GF 4 and Similar Grade Engine
Oils by Inductively Coupled Plasma Atomic Emission large reproducibility estimate or the data being dropped from
the study as an outlier.
Spectrometry
D7041 Test Method for Determination of Total Sulfur in
4.3 Uniform practice for sample preparation is beneficial in
LightHydrocarbons,MotorFuels,andOilsbyOnlineGas
standardizing the procedures and obtaining consistent results
Chromatography with Flame Photometric Detection
across the laboratories.
D7111 Test Method for Determination of Trace Elements in
Middle Distillate Fuels by Inductively Coupled Plasma 5. Gross Sample Preparation
Atomic Emission Spectrometry (ICP-AES)
5.1 Collection of a meaningful and representative sample is
D7171 Test Method for Hydrogen Content of Middle Dis-
often the most critical step in an analytical procedure. In trace
tillate Petroleum Products by Low-Resolution Pulsed
element analysis, in particular, extreme care must be taken to
Nuclear Magnetic Resonance Spectroscopy
avoidcontaminationofthesamplesduringthesamplingandall
D7212 Test Method for Low Sulfur inAutomotive Fuels by
subsequent analysis steps. Good laboratory practices in this
Energy-Dispersive X-ray Fluorescence Spectrometry Us-
area can include:
ing a Low-Background Proportional Counter
5.1.1 The sample received by the laboratory for analysis
D7220 Test Method for Sulfur in Automotive, Heating, and
needs to be stored in a designated specific storage location
Jet Fuels by Monochromatic Energy Dispersive X-ray
whileawaitinganalysis.Thisarea,wheneverpossible,shallnot
Fluorescence Spectrometry
contain materials with high levels of specific elements that
D7303 Test Method for Determination of Metals in Lubri-
couldcontaminateothersamplesrequiringtraceelementanaly-
cating Greases by Inductively Coupled Plasma Atomic
sis.
Emission Spectrometry
5.1.2 All laboratory equipment used specifically for trace
D7318 TestMethodforExistentInorganicSulfateinEthanol
element analysis need to be free of any source of contamina-
by Potentiometric Titration
tion.This may require that specific equipment be used only for
D7319 Test Method for Determination of Existent and Po-
trace element analysis.
tential Sulfate and Inorganic Chloride in Fuel Ethanol by
5.1.3 Use working surfaces that can be decontaminated
Direct Injection Suppressed Ion Chromatography
easily if a spillage occurs. The atmosphere needs to be free of
D7328 Test Method for Determination of Existent and Po-
interfering gases and dust particles.
tential Inorganic Sulfate and Total Inorganic Chloride in
5.1.4 Wear clean, fresh, protective, and impermeable gloves
Fuel Ethanol by Ion Chromatography Using Aqueous
for sample preparation for trace element analysis, appropriate
Sample Injection
for the materials being handled. Test the gloves to confirm that
WK16905 Practice for Sampling, Storage, and Handling of
theydonotcontaininterferingelementsorelementsofinterest,
Hydrocarbon Samples for Mercury Analysis
sincetheymaycausecontamination.Thedevelopmentofclean
area sample handling protocols is encouraged.
3. Summary of Practice
5.2 All laboratory samples should be collected in accor-
3.1 This practice covers alternate ways of preparing a
dance with Practices D4057 and D4177. The personnel col-
petroleum product or lubricant sample for elemental analysis
lecting the samples should be properly trained in sampling,
measurements. The means of preparation of samples may vary
since invalid sampling can lead to invalid results. The respon-
from no special steps to extensive detailed procedures depen- sibility of the laboratory starts on receipt of the sample in the
dentonthesamplematrixandthemeasurementtechniquetobe
laboratory.
used.
5.2.1 It would be useful for the laboratory personnel to
assist the plant personnel in securing a representative
3.2 This practice may also be applicable to non-petroleum
contamination-free sample. Often inappropriate or unclean
based biofuels. Work is underway to validate the applicability
containers are used to collect the samples in plant or field. It
to these types of materials.
would help if the laboratory can provide pre-cleaned sample
containers to the plant personnel collecting the samples.
4. Significance and Use
5.2.1.1 The clean container, lid, liner seal, and liner adhe-
4.1 Crudeoil,petroleum,petroleumproducts,additives,and sive shall not contaminate the sample, and the sample shall not
lubricants are routinely analyzed for their elemental content compromise the integrity of the container.
such as chlorine, nitrogen, phosphorus, sulfur, and various 5.2.1.2 Consult Department of Transportation packaging
metals using a variety of analytical techniques. Some of these guidelines or other appropriate sources, such as placing in a
test methods require little to no sample preparation; some Hazmat-Pak, taping caps in place after securing tightly
others require only simple dilutions; while others require container/liner compatibility, judicious use of vermiculite as a
elaborate sample decomposition before the product is analyzed packing material considering contamination as well as user
for its elemental content. safety from inhaled
...
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