ASTM D7455-19
(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
4.1 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.
4.2 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.
4.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.8 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.
General Information
- Status
- Published
- Publication Date
- 30-Apr-2019
- Technical Committee
- D02 - Petroleum Products, Liquid Fuels, and Lubricants
- Drafting Committee
- D02.03 - Elemental Analysis
Relations
- Effective Date
- 01-May-2019
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Nov-2023
- Effective Date
- 01-Nov-2023
- Effective Date
- 01-May-2020
- Effective Date
- 01-May-2020
- Effective Date
- 01-May-2020
- Effective Date
- 01-May-2020
- Effective Date
- 01-May-2020
- Effective Date
- 01-Jul-2019
- Effective Date
- 01-May-2019
- Effective Date
- 01-May-2019
Overview
ASTM D7455-19: Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis provides industry-wide guidance for preparing crude oil, petroleum, lubricant, additive, and bio-fuel samples for elemental analysis. This practice is essential for ensuring uniformity and reliability in the determination of key elements such as chlorine, nitrogen, phosphorus, sulfur, and various metals.
Proper sample preparation is fundamental to producing accurate and reproducible elemental analysis results. The standard covers a range of sample types and outlines basic preparation steps required by different analytical techniques, including cases that require no preparation, simple dilution, or more complex decomposition processes. It emphasizes that users should refer to individual test methods for any unique scenarios.
Key Topics
Sample Collection and Handling
- Use of contamination-free storage and sampling containers
- Appropriate protective measures and clean laboratory practices
- Training for personnel to prevent sampling errors
Preliminary Sample Treatment
- Homogenization techniques to ensure representative analysis
- Prevention of contamination from dust, equipment, or improper storage
Sample Preparation Techniques
- Procedures requiring:
- No sample preparation (e.g., many XRF methods)
- Solvent dilution for viscosity adjustment or matrix matching
- Ashing and sulfated ash methods for converting organics to inorganics
- Acid digestion or decomposition for complex matrices
- Combustion approaches for total sulfur, chlorine, or nitrogen
- Procedures requiring:
Contamination Control
- Recommendations for using inert, non-metallic containers (plastic, PTFE, glass)
- Screening solvents and reagents for trace contaminants
Special Considerations
- Handling of volatile or multi-phase samples, like stabilized crudes or fuels with particulate matter
- Application of the practice to non-petroleum bio-fuels
Applications
ASTM D7455-19 is widely used in laboratories and quality assurance settings for:
Routine Factory and Laboratory Testing:
Facilitating consistent sample preparation for elemental analysis of petroleum products, base oils, lubricants, and additives.Trace Element Detection:
Ensuring accurate results for elements that may impact product performance, regulatory compliance, or environmental impact.Inter-laboratory Consistency:
Enabling reproducible and comparable results across different laboratories by minimizing preparation-induced biases or errors.Research and Development:
Supporting new product development and benchmarking by producing high-integrity data for sample composition.Bio-fuels Analysis:
Extending best practices to emerging renewable fuel sectors as ongoing work within ASTM broadens applicability.
Related Standards
ASTM D7455-19 frequently references and complements various ASTM standards and test methods, including but not limited to:
Sampling and Storage:
- ASTM D4057: Manual Sampling of Petroleum and Petroleum Products
- ASTM D4177: Automatic Sampling of Petroleum and Petroleum Products
Elemental Analysis Methods:
- ASTM D4294: Sulfur Analysis by Energy Dispersive X-Ray Fluorescence (XRF)
- ASTM D4951, D5185: Inductively Coupled Plasma (ICP) for multielement analysis
- ASTM D2622: Sulfur by Wavelength Dispersive XRF
- ASTM D1091, D4047: Phosphorus in Lubricating Oils and Additives
Special Sample Preparation:
- ASTM C1234: High-Pressure, High-Temperature Digestion for Trace Elements
- ASTM D7876: Sample Decomposition Using Microwave Heating
- ASTM D7482: Sampling and Storage of Hydrocarbons for Mercury Analysis
Visit ASTM International for the full list of complementary standards relevant to petroleum and lubricant sample preparation for elemental analysis.
By using ASTM D7455-19, laboratories and industry stakeholders ensure their elemental analysis results are accurate, reliable, and aligned with global best practices for sample preparation of petroleum, lubricant, and bio-fuel products.
Buy Documents
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
REDLINE ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Get Certified
Connect with accredited certification bodies for this standard
ABS Quality Evaluations Inc.
American Bureau of Shipping quality certification.
Element Materials Technology
Materials testing and product certification.
ABS Group Brazil
ABS Group certification services in Brazil.
Sponsored listings
Frequently Asked Questions
ASTM D7455-19 is a standard published by ASTM International. Its full title is "Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis". This standard covers: SIGNIFICANCE AND USE 4.1 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. 4.2 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. 4.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.8 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.
SIGNIFICANCE AND USE 4.1 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. 4.2 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. 4.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.8 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.
ASTM D7455-19 is classified under the following ICS (International Classification for Standards) categories: 75.100 - Lubricants, industrial oils and related products. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D7455-19 has the following relationships with other standards: It is inter standard links to ASTM D7455-14, ASTM D6481-24, ASTM D3231-24, ASTM D86-23a, ASTM D86-23ae1, ASTM D4808-23, ASTM D3701-23, ASTM D7171-20, ASTM D6470-99(2020), ASTM D7620-10(2020), ASTM D7040-04(2020), ASTM D6732-04(2020), ASTM D5453-19a, ASTM D7260-19, ASTM D5384-14(2019). Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM D7455-19 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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: D7455 − 19
Standard Practice 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* mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This practice covers different means by which petro-
leumproductandlubricantsamplesmaybepreparedbeforethe
2. Referenced Documents
measurement of their elemental content using different analyti-
2.1 ASTM Standards:
cal techniques.
C1234 Practice for Preparation of Oils and Oily Waste
1.2 This practice includes only the basic steps for generally
Samples by High-Pressure, High-Temperature Digestion
encountered sample types. Anything out of the ordinary may
for Trace Element Determinations
require special procedures. See individual test methods for
D86 Test Method for Distillation of Petroleum Products and
instructions to handle such situations.
Liquid Fuels at Atmospheric Pressure
D129 Test Method for Sulfur in Petroleum Products (Gen-
1.3 This practice is not a substitute for a thorough under-
eral High Pressure Decomposition Device Method)
standing of the actual test method to be used, caveats the test
D482 Test Method for Ash from Petroleum Products
method contains, and additional sample preparation that may
D808 Test Method for Chlorine in New and Used Petroleum
be required.
Products (High Pressure Decomposition Device Method)
1.4 The user should not expand the scope of the test
D874 Test Method for Sulfated Ash from Lubricating Oils
methods to materials or concentrations outside the scope of the
and Additives
test methods being used without thoroughly understanding the
D1018 Test Method for Hydrogen In Petroleum Fractions
implications of such deviations.
D1091 Test Methods for Phosphorus in Lubricating Oils and
1.5 This practice may also be applicable to sample prepa-
Additives
ration of non-petroleum based bio-fuels for elemental analysis.
D1266 Test Method for Sulfur in Petroleum Products (Lamp
Currently,workisongoinginASTMSubcommitteeD02.03;as
Method)
information becomes available, it will be added to this stan-
D1318 Test Method for Sodium in Residual Fuel Oil (Flame
dard.
Photometric Method)
D1548 Test Method for Vanadium in Heavy Fuel Oil
1.6 The values stated in SI units are to be regarded as
(Withdrawn 1997)
standard. No other units of measurement are included in this
D1552 Test Method for Sulfur in Petroleum Products by
standard.
High Temperature Combustion and Infrared (IR) Detec-
1.7 This standard does not purport to address all of the
tion or Thermal Conductivity Detection (TCD)
safety concerns, if any, associated with its use. It is the
D2622 Test Method for Sulfur in Petroleum Products by
responsibility of the user of this standard to establish appro-
Wavelength Dispersive X-ray Fluorescence Spectrometry
priate safety, health, and environmental practices and deter-
D2784 Standard Test Method for Sulfur in Liquefied Petro-
mine the applicability of regulatory limitations prior to use.
leum Gases (Oxy-Hydrogen Burner or Lamp)(Withdrawn
1.8 This international standard was developed in accor-
2016)
dance with internationally recognized principles on standard-
D3120 Test Method for Trace Quantities of Sulfur in Light
ization established in the Decision on Principles for the
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
Development of International Standards, Guides and Recom-
lometry
1 2
This practice is under the jurisdiction ofASTM Committee D02 on Petroleum For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
mittee D02.03 on Elemental Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2019. Published May 2019. Originally the ASTM website.
approved in 2008. Last previous edition approved in 2014 as D7455 – 14. DOI: The last approved version of this historical standard is referenced on
10.1520/D7455-19. www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7455 − 19
D3228 Test Method for Total Nitrogen in Lubricating Oils Coupled Plasma Atomic Emission Spectrometry, and
and Fuel Oils by Modified Kjeldahl Method Atomic Absorption Spectrometry
D3230 Test Method for Salts in Crude Oil (Electrometric D5185 Test Method for Multielement Determination of
Method)
Used and Unused Lubricating Oils and Base Oils by
D3231 Test Method for Phosphorus in Gasoline
Inductively Coupled Plasma Atomic Emission Spectrom-
D3237 TestMethodforLeadinGasolinebyAtomicAbsorp-
etry (ICP-AES)
tion Spectroscopy
D5291 Test Methods for Instrumental Determination of
D3246 Test Method for Sulfur in Petroleum Gas by Oxida-
Carbon, Hydrogen, and Nitrogen in Petroleum Products
tive Microcoulometry
and Lubricants
D3340 Test Method for Lithium and Sodium in Lubricating
D5384 Test Methods for Chlorine in Used Petroleum Prod-
Greases by Flame Photometer (Withdrawn 2013)
ucts (Field Test Kit Method)
D3341 Test Method for Lead in Gasoline—Iodine Mono-
D5453 Test Method for Determination of Total Sulfur in
chloride Method
Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel
D3348 Test Method for Rapid Field Test for Trace Lead in
Engine Fuel, and Engine Oil by Ultraviolet Fluorescence
Unleaded Gasoline (Colorimetric Method)
D5600 Test Method for Trace Metals in Petroleum Coke by
D3605 Test Method for Trace Metals in Gas Turbine Fuels
Inductively Coupled Plasma Atomic Emission Spectrom-
by Atomic Absorption and Flame Emission Spectroscopy
etry (ICP-AES)
D3701 Test Method for Hydrogen Content of Aviation
D5622 Test Methods for Determination of Total Oxygen in
Turbine Fuels by Low Resolution Nuclear Magnetic
Gasoline and Methanol Fuels by Reductive Pyrolysis
Resonance Spectrometry
D5708 Test Methods for Determination of Nickel,
D3831 Test Method for Manganese in Gasoline By Atomic
Vanadium, and Iron in Crude Oils and Residual Fuels by
Absorption Spectroscopy
Inductively Coupled Plasma (ICP) Atomic Emission
D4045 Test Method for Sulfur in Petroleum Products by
Spectrometry
Hydrogenolysis and Rateometric Colorimetry
D5762 Test Method for Nitrogen in Liquid Hydrocarbons,
D4047 Test Method for Phosphorus in Lubricating Oils and
Petroleum and Petroleum Products by Boat-Inlet Chemi-
Additives by Quinoline Phosphomolybdate Method
luminescence
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 Hydrocar-
D6445 Test Method for Sulfur in Gasoline by Energy-
bons by Syringe/Inlet Oxidative Combustion and Chemi-
Dispersive X-ray Fluorescence Spectrometry (Withdrawn
luminescence 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 Method 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
D5059 Test Methods for Lead in Gasoline by X-Ray Spec- Electrode Atomic Emission Spectrometry
troscopy D6732 Test Method for Determination of Copper in Jet
Fuels by Graphite Furnace Atomic Absorption Spectrom-
D5184 Test Methods for Determination of Aluminum and
Silicon in Fuel Oils by Ashing, Fusion, Inductively etry
D7455 − 19
D6920 Test Method forTotal Sulfur in Naphthas, Distillates, D7623 Test Method for Total Mercury in Crude Oil Using
Reformulated Gasolines, Diesels, Biodiesels, and Motor Combustion-GoldAmalgamation and Cold VaporAtomic
Absorption Method
Fuels by Oxidative Combustion and Electrochemical De-
D7691 TestMethodforMultielementAnalysisofCrudeOils
tection (Withdrawn 2018)
Using Inductively Coupled Plasma Atomic Emission
D7039 Test Method for Sulfur in Gasoline, Diesel Fuel, Jet
Spectrometry (ICP-AES)
Fuel, Kerosine, Biodiesel, Biodiesel Blends, and
D7740 Practice for Optimization, Calibration, and Valida-
Gasoline-Ethanol Blends by Monochromatic Wavelength
tion ofAtomicAbsorption Spectrometry for MetalAnaly-
Dispersive X-ray Fluorescence Spectrometry
sis of Petroleum Products and Lubricants
D7040 Test Method for Determination of Low Levels of
D7751 Test Method for Determination ofAdditive Elements
Phosphorus in ILSAC GF 4 and Similar Grade Engine
in Lubricating Oils by EDXRF Analysis
Oils by Inductively Coupled Plasma Atomic Emission
D7757 Test Method for Silicon in Gasoline and Related
Spectrometry
Products by Monochromatic Wavelength Dispersive
D7041 Test Method for Determination of Total Sulfur in
X-ray Fluorescence Spectrometry
Liquid Hydrocarbons and Hydrocarbon-Oxygenate
D7876 Practice for Practice for Sample Decomposition Us-
Blends by Gas Chromatography with Flame Photometric
ing Microwave Heating (With or Without Prior Ashing)
Detection
for Atomic Spectroscopic Elemental Determination in
D7111 Test Method for Determination of Trace Elements in
Petroleum Products and Lubricants
Middle Distillate Fuels by Inductively Coupled Plasma
D8110 Test Method for Elemental Analysis of Distillate
Atomic Emission Spectrometry (ICP-AES)
Products by Inductively Coupled Plasma Mass Spectrom-
D7171 Test Method for Hydrogen Content of Middle Dis-
etry (ICP-MS)
tillate Petroleum Products by Low-Resolution Pulsed
D8127 Test Method for Coupled Particulate and Elemental
Nuclear Magnetic Resonance Spectroscopy
Analysis using X-ray Fluorescence (XRF) for In-Service
D7212 Test Method for Low Sulfur inAutomotive Fuels by
Lubricants
Energy-Dispersive X-ray Fluorescence Spectrometry Us-
D8150 Test Method for Determination of Organic Chloride
ing a Low-Background Proportional Counter
Content in Crude Oil by Distillation Followed by Detec-
D7220 Test Method for Sulfur in Automotive, Heating, and
tion Using Combustion Ion Chromatography
Jet Fuels by Monochromatic Energy Dispersive X-ray
3. Summary of Practice
Fluorescence Spectrometry
3.1 This practice covers alternative ways of preparing a
D7260 Practice for Optimization, Calibration, and Valida-
petroleum product or lubricant sample for elemental analysis
tion of Inductively Coupled Plasma-Atomic Emission
measurements. The means of preparation of samples may vary
Spectrometry (ICP-AES) for ElementalAnalysis of Petro-
from no special steps to extensive detailed procedures depen-
leum Products and Lubricants
dentonthesamplematrixandthemeasurementtechniquetobe
D7303 Test Method for Determination of Metals in Lubri-
used.
cating Greases by Inductively Coupled Plasma Atomic
Emission Spectrometry
3.2 This practice may also be applicable to non-petroleum
D7318 TestMethodforExistentInorganicSulfateinEthanol based biofuels. Work is underway to validate the applicability
by Potentiometric Titration to these types of materials.
D7319 Test Method for Determination of Existent and Po-
4. Significance and Use
tential Sulfate and Inorganic Chloride in Fuel Ethanol and
4.1 Crudeoil,petroleum,petroleumproducts,additives,and
Butanol by Direct Injection Suppressed Ion Chromatog-
lubricants are routinely analyzed for their elemental content
raphy
such as chlorine, nitrogen, phosphorus, sulfur, and various
D7328 Test Method for Determination of Existent and Po-
metals using a variety of analytical techniques. Some of these
tential Inorganic Sulfate and Total Inorganic Chloride in
test methods require little to no sample preparation; some
Fuel Ethanol by Ion Chromatography Using Aqueous
others require only simple dilutions; while others require
Sample Injection
elaborate sample decomposition before the product is analyzed
D7343 Practice for Optimization, Sample Handling,
for its elemental content.
Calibration, and Validation of X-ray Fluorescence Spec-
4.2 Fairly often it can be shown that the round robin results
trometry Methods for Elemental Analysis of Petroleum
by a co-operator are all biased with respect to those from other
Products and Lubricants
laboratories. Presumably, the failure to follow good laboratory
D7482 Practice for Sampling, Storage, and Handling of
practices and instructions in the test methods can be a causal
Hydrocarbons for Mercury Analysis
factorofsucherrors.Afurtherconsequenceisanunnecessarily
D7620 Test Method for Determination of Total Sulfur in
large reproducibility estimate or the data being dropped from
LiquidHydrocarbonBasedFuelsbyContinuousInjection,
the study as an outlier.
Air Oxidation and Ultraviolet Fluorescence Detection
D7622 Test Method for Total Mercury in Crude Oil Using 4.3 Uniform practice for sample preparation is beneficial in
Combustion and Direct Cold Vapor Atomic Absorption
standardizing the procedures and obtaining consistent results
Method with Zeeman Background Correction across the laboratories.
D7455 − 19
5. Gross Sample Preparation shaker. Purge the sampling port lines on tanks properly before
collecting the samples.
5.1 Collection of a meaningful and representative sample is
often the most critical step in an analytical procedure. In trace
5.4 Care must be taken during the homogenization proce-
element analysis, in particular, extreme care must be taken to durethatthesampleisnotcontaminatedwithdust,particles,or
avoidcontaminationofthesamplesduringthesamplingandall
by contact with other sources of metals.
subsequent analysis steps. Good laboratory practices in this
5.4.1 Stabilizedcrudeoilstypicallycontainmultiplephases,
area can include:
particulates, and volatiles. Decisions whether to separate the
5.1.1 The sample received by the laboratory for analysis
phases and analyze them separately, or homogenize the whole
needs to be stored in a designated specific storage location
sample need to be made prior to analysis.
whileawaitinganalysis.Thisarea,wheneverpossible,shallnot
5.5 Many samples contain volatile components. Hence, it is
contain materials with high levels of specific elements that
prudenttokeepthesamplerefrigerateduntilreadyforanalysis.
couldcontaminateothersamplesrequiringtraceelementanaly-
This is particularly true for products such as gasoline, diesel,
sis.
reformulated gasoline, jet fuel, etc. Vessel pressure integrity
5.1.2 All laboratory equipment used specifically for trace
and permeability need to be considered.
element analysis need to be free of any source of contamina-
5.5.1 Unlessagiventestmethodprocedurestatesotherwise,
tion.This may require that specific equipment be used only for
refrigerated samples should be warmed to ambient temperature
trace element analysis.
before taking an aliquot for analysis. During warming, con-
5.1.3 Use working surfaces that can be decontaminated
densation of moisture on the sample containers is a concern.
easily if a spillage occurs. The atmosphere needs to be free of
5.5.2 Potential overpressure hazard, just like heating a
interfering gases and dust particles.
sealed container in an oven needs to be lessened by loosening
5.1.4 Wear clean, fresh, protective, and impermeable gloves
the cap to prevent rupture. However, this can result in loss of
for sample preparation for trace element analysis, appropriate
light ends, depending on the material composition.
for the materials being handled. Test the gloves to confirm that
5.5.3 If the sample does not readily flow at room
theydonotcontaininterferingelementsorelementsofinterest,
temperature, heat it to a sufficiently high and safe temperature
sincetheymaycausecontamination.Thedevelopmentofclean
to ensure adequate fluidity.
area sample handling protocols is encouraged.
5.5.4 Greatcareneedstobeexercisedinheatingtheviscous
5.2 All laboratory samples should be collected in accor-
samples prior to analysis. Changes in chemical composition,
dance with Practices D4057 and D4177. The personnel col-
loss of volatile elements, etc. are causes for concern.
lecting the samples should be properly trained in sampling,
5.6 Fuel samples can contain particulate matter and free
since invalid sampling can lead to invalid results. The respon-
water. In order to be representative, always shake vigorously
sibility of the laboratory starts on receipt of the sample in the
prior to taking a test specimen for analysis.
laboratory.
5.6.1 Samples that have been in transit for several days, idle
5.2.1 It would be useful for the laboratory personnel to
in storage, or viscous may be placed in a heated ultrasonic bath
assist the plant personnel in securing a representative
to break up clusters of particles and to bring them back into
contamination-free sample. Often inappropriate or unclean
suspension. The samples may be vigorously shaken with a
containers are used to collect the samples in plant or field. It
power mixer after being in an ultrasonic bath and prior to
would help if the laboratory can provide pre-cleaned sample
pouring a test specimen for analysis. The bath temperature
containers to the plant personnel collecting the samples.
should be 60 °C for very viscous fuels and below the flash
5.2.1.1 The clean container, lid, liner seal, and liner adhe-
point for non-viscous fuels. The total agitation time for a
sive shall not contaminate the sample, and the sample shall not
sample should be at least 2 min.
compromise the integrity of the container.
5.6.2 Impeller mixers can be a source of contamination as
5.2.1.2 Consult Department of Transportation packaging
well.Air-drivenmotors(forexample,oilordust),bearingwear
guidelines or other appropriate sources, such as placing in a
contaminants, leaching of metals from impellers, impeller
Hazmat-Pak, taping caps in place after securing tightly
abrasioncontactwithcontainer,etc.,aresomeofthepointsthat
container/liner compatibility, judicious use of vermiculite as a
need to be thought of as potential contamination sources.
packing material considering contamination as well as user
5.6.3 From a safety perspective, electric motors present an
safety from inhaled dust, etc.
ignition hazard with flammables. Long term use of ultrasonic
5.2.2 To preserve sample integrity and prevent the loss of
baths can overheat samples. To prevent fire or explosion, an
volatile components, which can be present in some samples,
operator should always remain present during these prepara-
they shall not be kept uncovered any longer than necessary.
tions and never leave any of these operations unattended.
Samples need to be analyzed as soon as possible after taking
from the bulk supplies to prevent loss of volatile species or
contamination. 6. Contamination Control
5.3 Before taking an aliquot of the bulk sample, ensure that 6.1 Samples that are used for the determination of metals
the sample is well-mixed and homogenous. This can be shall be scrupulously kept away from contact with metal
ensured, if necessary, by the use of an ultrasonic device or containers and laboratory utensils. Wherever possible, plastic
vigorously stirring with a magnetic or mechanical stirrer or or other inert materials shall be used.
D7455 − 19
6.2 Reagents and solvents used in chemical processing of 8. Methods Requiring Solvent Dilution
the samples need to be free of trace elements. For example,
8.1 For several test methods, the only sample preparation
laboratory wipe tissues commonly used in many laboratories
required is a simple dilution with appropriate organic solvent.
for wiping laboratory glassware has been reported to contain
Most of these test methods are based on atomic absorption
48 ppm of zinc, and could be a potential source of contamina-
spectrometry (AAS) or inductively coupled plasma atomic
tion.
emission spectrometry (ICP-AES) measurement of analytes of
6.3 Trace elements in the sample can interact with the wall interest.Thereasonforthisstepcouldbethateitherthesample
containers and subsequently will result in low biased results. is too viscous to flow through the nebulizer or the viscosity of
On the other hand, if the sample matrix is reacting with the the sample needs to match that of the calibration standards. In
containers, metals will leach out in the sample leading to high both cases this is achieved by appropriate dilution with an
biased results. However, in both cases, the results will not organic solvent or a solvent mixture.
represent the true elemental concentration in the original
8.2 A variety of organic solvents have been used for this
sample.
purpose: methyl iso-butyl ketone, heavy distillate, kerosene,
6.4 Acid-washed glass containers lined with inert sub-
xylenes, acetone, etc.
stances and polyethylene-polypropylene-PTFE, or both, con-
8.3 The test methods that require such solvent dilutions
tainersarethebestcontainersforstorageofpetroleump
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D7455 − 14 D7455 − 19
Standard Practice 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*
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.8 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.
2. Referenced Documents
2.1 ASTM Standards:
C1234 Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace
Element Determinations
D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
D129 Test Method for Sulfur in Petroleum Products (General High Pressure Decomposition Device Method)
D482 Test Method for Ash from Petroleum Products
D808 Test Method for Chlorine in New and Used Petroleum Products (High Pressure Decomposition Device Method)
D874 Test Method for Sulfated Ash from Lubricating Oils and Additives
D1018 Test Method for Hydrogen In Petroleum Fractions
D1091 Test Methods for Phosphorus in Lubricating Oils and Additives
D1266 Test Method for Sulfur in Petroleum Products (Lamp Method)
D1318 Test Method for Sodium in Residual Fuel Oil (Flame Photometric Method)
1 3
D1548 Test Method for Vanadium in Heavy Fuel Oil (Withdrawn 1997)
This practice is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
Current edition approved May 1, 2014May 1, 2019. Published May 2014May 2019. Originally approved in 2008. Last previous edition approved in 20082014 as
D7455 – 08.D7455 – 14. DOI: 10.1520/D7455-14.10.1520/D7455-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7455 − 19
D1552 Test Method for Sulfur in Petroleum Products by High Temperature Combustion and Infrared (IR) Detection or Thermal
Conductivity Detection (TCD)
D2622 Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry
D2784 Standard Test Method for Sulfur in Liquefied Petroleum Gases (Oxy-Hydrogen Burner or Lamp) (Withdrawn 2016)
D3120 Test Method for Trace Quantities of Sulfur in Light Liquid Petroleum Hydrocarbons by Oxidative Microcoulometry
D3228 Test Method for Total Nitrogen in Lubricating Oils and Fuel Oils by Modified Kjeldahl Method
D3230 Test Method for Salts in Crude Oil (Electrometric Method)
D3231 Test Method for Phosphorus in Gasoline
D3237 Test Method for Lead in Gasoline by Atomic Absorption Spectroscopy
D3246 Test Method for Sulfur in Petroleum Gas by Oxidative Microcoulometry
D3340 Test Method for Lithium and Sodium in Lubricating Greases by Flame Photometer (Withdrawn 2013)
D3341 Test Method for Lead in Gasoline—Iodine Monochloride Method
D3348 Test Method for Rapid Field Test for Trace Lead in Unleaded Gasoline (Colorimetric Method)
D3605 Test Method for Trace Metals in Gas Turbine Fuels by Atomic Absorption and Flame Emission Spectroscopy
D3701 Test Method for Hydrogen Content of Aviation Turbine Fuels by Low Resolution Nuclear Magnetic Resonance
Spectrometry
D3831 Test Method for Manganese in Gasoline By Atomic Absorption Spectroscopy
D4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
D4047 Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4294 Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry
D4628 Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption
Spectrometry
D4629 Test Method for Trace Nitrogen in Liquid Hydrocarbons by Syringe/Inlet Oxidative Combustion and Chemiluminescence
Detection
D4808 Test Methods for Hydrogen Content of Light Distillates, Middle Distillates, Gas Oils, and Residua by Low-Resolution
Nuclear Magnetic Resonance Spectroscopy
D4927 Test Methods for Elemental Analysis of Lubricant and Additive Components—Barium, Calcium, Phosphorus, Sulfur,
and Zinc by Wavelength-Dispersive X-Ray Fluorescence Spectroscopy
D4929 Test Method for Determination of Organic Chloride Content in Crude Oil
D4951 Test Method for Determination of Additive Elements in Lubricating Oils by Inductively Coupled Plasma Atomic
Emission Spectrometry
D5056 Test Method for Trace Metals in Petroleum Coke by Atomic Absorption
D5059 Test Methods for Lead in Gasoline by X-Ray Spectroscopy
D5184 Test Methods for Determination of Aluminum and Silicon in Fuel Oils by Ashing, Fusion, Inductively Coupled Plasma
Atomic Emission Spectrometry, and Atomic Absorption Spectrometry
D5185 Test Method for Multielement Determination of Used and Unused Lubricating Oils and Base Oils by Inductively
Coupled Plasma Atomic Emission Spectrometry (ICP-AES)
D5291 Test Methods for Instrumental Determination of Carbon, Hydrogen, and Nitrogen in Petroleum Products and Lubricants
D5384 Test Methods for Chlorine in Used Petroleum Products (Field Test Kit Method)
D5453 Test Method for Determination of Total Sulfur in Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel Engine Fuel,
and Engine Oil by Ultraviolet Fluorescence
D5600 Test Method for Trace Metals in Petroleum Coke by Inductively Coupled Plasma Atomic Emission Spectrometry
(ICP-AES)
D5622 Test Methods for Determination of Total Oxygen in Gasoline and Methanol Fuels by Reductive Pyrolysis
D5708 Test Methods for Determination of Nickel, Vanadium, and Iron in Crude Oils and Residual Fuels by Inductively Coupled
Plasma (ICP) Atomic Emission Spectrometry
D5762 Test Method for Nitrogen in Liquid Hydrocarbons, Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence
D5863 Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame
Atomic Absorption Spectrometry
D6334 Test Method for Sulfur in Gasoline by Wavelength Dispersive X-Ray Fluorescence
D6443 Test Method for Determination of Calcium, Chlorine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in Unused
Lubricating Oils and Additives by Wavelength Dispersive X-ray Fluorescence Spectrometry (Mathematical Correction
Procedure)
D6445 Test Method for Sulfur in Gasoline by Energy-Dispersive X-ray Fluorescence Spectrometry (Withdrawn 2009)
D6470 Test Method for Salt in Crude Oils (Potentiometric Method)
D7455 − 19
D6481 Test Method for Determination of Phosphorus, Sulfur, Calcium, and Zinc in Lubrication Oils by Energy Dispersive X-ray
Fluorescence Spectroscopy
D6595 Test Method for Determination of Wear Metals and Contaminants in Used Lubricating Oils or Used Hydraulic Fluids by
Rotating Disc Electrode Atomic Emission Spectrometry
D6667 Test Method for Determination of Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by
Ultraviolet Fluorescence
D6728 Test Method for Determination of Contaminants in Gas Turbine and Diesel Engine Fuel by Rotating Disc Electrode
Atomic Emission Spectrometry
D6732 Test Method for Determination of Copper in Jet Fuels by Graphite Furnace Atomic Absorption Spectrometry
D6920 Test Method for Total Sulfur in Naphthas, Distillates, Reformulated Gasolines, Diesels, Biodiesels, and Motor Fuels by
Oxidative Combustion and Electrochemical Detection (Withdrawn 2018)
D7039 Test Method for Sulfur in Gasoline, Diesel Fuel, Jet Fuel, Kerosine, Biodiesel, Biodiesel Blends, and Gasoline-Ethanol
Blends by Monochromatic Wavelength Dispersive X-ray Fluorescence Spectrometry
D7040 Test Method for Determination of Low Levels of Phosphorus in ILSAC GF 4 and Similar Grade Engine Oils by
Inductively Coupled Plasma Atomic Emission Spectrometry
D7041 Test Method for Determination of Total Sulfur in Liquid Hydrocarbons and Hydrocarbon-Oxygenate Blends by Gas
Chromatography with Flame Photometric Detection
D7111 Test Method for Determination of Trace Elements in Middle Distillate Fuels by Inductively Coupled Plasma Atomic
Emission Spectrometry (ICP-AES)
D7171 Test Method for Hydrogen Content of Middle Distillate Petroleum Products by Low-Resolution Pulsed Nuclear Magnetic
Resonance Spectroscopy
D7212 Test Method for Low Sulfur in Automotive Fuels by Energy-Dispersive X-ray Fluorescence Spectrometry Using a
Low-Background Proportional Counter
D7220 Test Method for Sulfur in Automotive, Heating, and Jet Fuels by Monochromatic Energy Dispersive X-ray Fluorescence
Spectrometry
D7260 Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry
(ICP-AES) for Elemental Analysis of Petroleum Products and Lubricants
D7303 Test Method for Determination of Metals in Lubricating Greases by Inductively Coupled Plasma Atomic Emission
Spectrometry
D7318 Test Method for Existent Inorganic Sulfate in Ethanol by Potentiometric Titration
D7319 Test Method for Determination of Existent and Potential Sulfate and Inorganic Chloride in Fuel Ethanol and Butanol by
Direct Injection Suppressed Ion Chromatography
D7328 Test Method for Determination of Existent and Potential Inorganic Sulfate and Total Inorganic Chloride in Fuel Ethanol
by Ion Chromatography Using Aqueous Sample Injection
D7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods
for Elemental Analysis of Petroleum Products and Lubricants
D7482 Practice for Sampling, Storage, and Handling of Hydrocarbons for Mercury Analysis
D7620 Test Method for Determination of Total Sulfur in Liquid Hydrocarbon Based Fuels by Continuous Injection, Air
Oxidation and Ultraviolet Fluorescence Detection
D7622 Test Method for Total Mercury in Crude Oil Using Combustion and Direct Cold Vapor Atomic Absorption Method with
Zeeman Background Correction
D7623 Test Method for Total Mercury in Crude Oil Using Combustion-Gold Amalgamation and Cold Vapor Atomic Absorption
Method
D7691 Test Method for Multielement Analysis of Crude Oils Using Inductively Coupled Plasma Atomic Emission Spectrometry
(ICP-AES)
D7740 Practice for Optimization, Calibration, and Validation of Atomic Absorption Spectrometry for Metal Analysis of
Petroleum Products and Lubricants
D7751 Test Method for Determination of Additive Elements in Lubricating Oils by EDXRF Analysis
D7757 Test Method for Silicon in Gasoline and Related Products by Monochromatic Wavelength Dispersive X-ray Fluorescence
Spectrometry
D7876 Practice for Practice for Sample Decomposition Using Microwave Heating (With or Without Prior Ashing) for Atomic
Spectroscopic Elemental Determination in Petroleum Products and Lubricants
D8110 Test Method for Elemental Analysis of Distillate Products by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
D8127 Test Method for Coupled Particulate and Elemental Analysis using X-ray Fluorescence (XRF) for In-Service Lubricants
D8150 Test Method for Determination of Organic Chloride Content in Crude Oil by Distillation Followed by Detection Using
Combustion Ion Chromatography
D7455 − 19
3. Summary of Practice
3.1 This practice covers alternatealternative ways of preparing a petroleum product or lubricant sample for elemental analysis
measurements. The means of preparation of samples may vary from no special steps to extensive detailed procedures dependent
on the sample matrix and the measurement technique to be used.
3.2 This practice may also be applicable to non-petroleum based biofuels. Work is underway to validate the applicability to these
types of materials.
4. Significance and Use
4.1 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.
4.2 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.
4.3 Uniform practice for sample preparation is beneficial in standardizing the procedures and obtaining consistent results across
the laboratories.
5. Gross Sample Preparation
5.1 Collection of a meaningful and representative sample is often the most critical step in an analytical procedure. In trace
element analysis, in particular, extreme care must be taken to avoid contamination of the samples during the sampling and all
subsequent analysis steps. Good laboratory practices in this area can include:
5.1.1 The sample received by the laboratory for analysis needs to be stored in a designated specific storage location while
awaiting analysis. This area, whenever possible, shall not contain materials with high levels of specific elements that could
contaminate other samples requiring trace element analysis.
5.1.2 All laboratory equipment used specifically for trace element analysis need to be free of any source of contamination. This
may require that specific equipment be used only for trace element analysis.
5.1.3 Use working surfaces that can be decontaminated easily if a spillage occurs. The atmosphere needs to be free of interfering
gases and dust particles.
5.1.4 Wear clean, fresh, protective, and impermeable gloves for sample preparation for trace element analysis, appropriate for
the materials being handled. Test the gloves to confirm that they do not contain interfering elements or elements of interest, since
they may cause contamination. The development of clean area sample handling protocols is encouraged.
5.2 All laboratory samples should be collected in accordance with Practices D4057 and D4177. The personnel collecting the
samples should be properly trained in sampling, since invalid sampling can lead to invalid results. The responsibility of the
laboratory starts on receipt of the sample in the laboratory.
5.2.1 It would be useful for the laboratory personnel to assist the plant personnel in securing a representative contamination-free
sample. Often inappropriate or unclean containers are used to collect the samples in plant or field. It would help if the laboratory
can provide pre-cleaned sample containers to the plant personnel collecting the samples.
5.2.1.1 The clean container, lid, liner seal, and liner adhesive shall not contaminate the sample, and the sample shall not
compromise the integrity of the container.
5.2.1.2 Consult Department of Transportation packaging guidelines or other appropriate sources, such as placing in a
Hazmat-Pak, taping caps in place after securing tightly container/liner compatibility, judicious use of vermiculite as a packing
material considering contamination as well as user safety from inhaled dust, etc.
5.2.2 To preserve sample integrity and prevent the loss of volatile components, which can be present in some samples, they shall
not be kept uncovered any longer than necessary. Samples need to be analyzed as soon as possible after taking from the bulk
supplies to prevent loss of volatile species or contamination.
5.3 Before taking an aliquot of the bulk sample, ensure that the sample is well-mixed and homogenous. This can be ensured,
if necessary, by the use of an ultrasonic device or vigorously stirring with a magnetic or mechanical stirrer or shaker. Purge the
sampling port lines on tanks properly before collecting the samples.
5.4 Care must be taken during the homogenization procedure that the sample is not contaminated with dust, particles, or by
contact with other sources of metals.
5.4.1 Stabilized crude oils typically contain multiple phases, particulates, and volatiles. Decisions whether to separate the phases
and analyze them separately, or homogenize the whole sample need to be made prior to analysis.
D7455 − 19
5.5 Many samples contain volatile components. Hence, it is prudent to keep the sample refrigerated until ready for analysis. This
is particularly true for products such as gasoline, diesel, reformulated gasoline, jet fuel, etc. Vessel pressure integrity and
permeability need to be considered.
5.5.1 Unless a given test method procedure states otherwise, refrigerated samples should be warmed to ambient temperature
before taking an aliquot for analysis. During warming, condensation of moisture on the sample containers is a concern.
5.5.2 Potential overpressure hazard, just like heating a sealed container in an oven needs to be lessened by loosening the cap
to prevent rupture. However, this can result in loss of light ends, depending on the material composition.
5.5.3 If the sample does not readily flow at room temperature, heat it to a sufficiently high and safe temperature to ensure
adequate fluidity.
5.5.4 Great care needs to be exercised in heating the viscous samples prior to analysis. Changes in chemical composition, loss
of volatile elements, etc. are causes for concern.
5.6 Fuel samples can contain particulate matter and free water. In order to be representative, always shake vigorously prior to
taking a test specimen for analysis.
5.6.1 Samples that have been in transit for several days, idle in storage, or viscous may be placed in a heated ultrasonic bath
to break up clusters of particles and to bring them back into suspension. The samples may be vigorously shaken with a power mixer
after being in an ultrasonic bath and prior to pouring a test specimen for analysis. The bath temperature should be 60°C60 °C for
very viscous fuels and below the flash point for non-viscous fuels. The total agitation time for a sample should be at least 2
min.2 min.
5.6.2 Impeller mixers can be a source of contamination as well. Air-driven motors (for example, oil or dust), bearing wear
contaminants, leaching of metals from impellers, impeller abrasion contact with container, etc., are some of the points that need
to be thought of as potential contamination sources.
5.6.3 From a safety perspective, electric motors present an ignition hazard with flammables. Long term use of ultrasonic baths
can overheat samples. To prevent fire or explosion, an operator should always remain present during these preparations and never
leave any of these operations unattended.
6. Contamination Control
6.1 Samples that are used for the determination of metals shall be scrupulously kept away from contact with metal containers
and laboratory utensils. Wherever possible, plastic or other inert materials shall be used.
6.2 Reagents and solvents used in chemical processing of the samples need to be free of trace elements. For example, laboratory
wipe tissues commonly used in many laboratories for wiping laboratory glassware has been reported to contain 48 ppm 48 ppm
of zinc, and could be a potential source of contamination.
6.3 Trace elements in the sample can interact with the wall containers and subsequently will result in low biased results. On
the other hand, if the sample matrix is reacting with the containers, metals will leach out in the sample leading to high biased
results. However, in both cases, the results will not represent the true elemental concentration in the original sample.
6.4 Acid-washed glass containers lined with inert substances and polyethylene-polypropylene-PTFE, or both, containers are the
best containers for storage of petroleum products and lubricants.
6.5 Materials used in dilutions, solubilizations, or adjusting pH, etc. need to be screened for possible contamination, especially
in trace element analysis.
7. Methods Requiring No Sample Preparation
7.1 There are a number of test methods that essentially require no sample preparation. Mostly these test methods are X-ray
fluorescence (XRF) test methods, and they include Test Methods D2622, D4294, D6334, D6445, D7039, D7212, and D7220 for
sulfur; Test Methods D3348 and D5059 for lead; Test Method D3605 for trace metals; and Test Methods D6443 and D6481 for
metals, and Test Method D7751 for additive elements in lubricating oils.oils; and Test Method D8127 for coupled particulate, and
iron and copper in-service lubricants.
7.1.1 However, in some procedures such as D2622, dilution is needed for samples containing >4.6 m% sulfur or for samples
containing >5 m% oxygen or other metals. Similarly, in Test Method D4294, it may be necessary to remove certain in
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...