ASTM D7578-10
(Guide)Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
SIGNIFICANCE AND USE
Crude oil, petroleum, petroleum products, additives, biofuels, and lubricants are routinely analyzed for their elemental content such as chlorine, nitrogen, hydrogen, phosphorus, sulfur, and various metals using a variety of analytical techniques. Some of these methods require little to no method calibration; some others require only simple one step calibration; while others require elaborate calibration routine 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.
Another cause of such discrepancies could be different or inadequate calibration practice used in the laboratory. Most test methods spell out the calibration requirements but often do not quote the frequency required letting the laboratories use good laboratory practices for this task. Thus, uniform practice for instrument calibration would be beneficial in standardizing the test procedures and obtaining consistent results across the laboratories.
Committee D02 has already issued standard practices for uniform sample preparation (D7455), standard operating procedures for ICP-AES (D7260) and XRF (D7343) as well as standard quality assurance protocol (D6792). This guide should be considered as a continuing effort on behalf of this subcommittee to achieve standardized practices in all parts of an analytical sequence.
SCOPE
1.1 This guide covers different ways by which the test methods used for elemental analysis of petroleum product and lubricant samples are calibrated before the sample analysis.
1.2 Uniform practice for test method calibration is beneficial in standardizing the procedures, and obtaining consistent results across different laboratories.
1.3 This guide includes only the basic steps for generally encountered instrument types. Anything out of the ordinary may require special procedures. See individual test methods for instructions to handle such situations.
1.4 This guide is not a substitute for a thorough understanding of the actual test method to be used, caveats it contains, and additional instrument preparation that may be required.
1.5 The user should not expand the scope of the test methods to materials or concentrations outside the scope of the test methods being used.
1.6 This guide should also be applicable to sample preparation of non-petroleum based bio-fuels for elemental analysis. Work is underway on these aspects in Subcommittee D02.03. As more information becomes available, it will be added to this standard.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 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: D7578 – 10
Standard Guide for
Calibration Requirements for Elemental Analysis of
Petroleum Products and Lubricants
This standard is issued under the fixed designation D7578; 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 D129 Test Method for Sulfur in Petroleum Products (Gen-
eral Bomb Method)
1.1 This guide covers different ways by which the test
D445 Test Method for Kinematic Viscosity of Transparent
methods used for elemental analysis of petroleum product and
and Opaque Liquids (and Calculation of Dynamic Viscos-
lubricant samples are calibrated before the sample analysis.
ity)
1.2 Uniform practice for test method calibration is benefi-
D482 Test Method for Ash from Petroleum Products
cial in standardizing the procedures, and obtaining consistent
D808 TestMethodforChlorineinNewandUsedPetroleum
results across different laboratories.
Products (Bomb Method)
1.3 This guide includes only the basic steps for generally
D874 Test Method for Sulfated Ash from Lubricating Oils
encountered instrument types. Anything out of the ordinary
and Additives
mayrequirespecialprocedures.Seeindividualtestmethodsfor
D892 Test Method for Foaming Characteristics of Lubricat-
instructions to handle such situations.
ing Oils
1.4 This guide is not a substitute for a thorough understand-
D1018 Test Method for Hydrogen In Petroleum Fractions
ingoftheactualtestmethodtobeused,caveatsitcontains,and
D1091 Test Methods for Phosphorus in Lubricating Oils
additional instrument preparation that may be required.
and Additives
1.5 The user should not expand the scope of the test
D1266 Test Method for Sulfur in Petroleum Products
methods to materials or concentrations outside the scope of the
(Lamp Method)
test methods being used.
D1318 TestMethodforSodiuminResidualFuelOil(Flame
1.6 This guide should also be applicable to sample prepa-
Photometric Method)
ration of non-petroleum based bio-fuels for elemental analysis.
D1548 Test Method for Vanadium in Navy Special Fuel
Work is underway on these aspects in Subcommittee D02.03.
Oil
Asmoreinformationbecomesavailable,itwillbeaddedtothis
D1552 Test Method for Sulfur in Petroleum Products
standard.
(High-Temperature Method)
1.7 The values stated in SI units are to be regarded as
D1839 Test Method for Amyl Nitrate in Diesel Fuels
standard. No other units of measurement are included in this
D2622 Test Method for Sulfur in Petroleum Products by
standard.
Wavelength Dispersive X-ray Fluorescence Spectrometry
1.8 This standard does not purport to address all of the
D2784 Test Method for Sulfur in Liquefied Petroleum
safety concerns, if any, associated with its use. It is the
Gases (Oxy-Hydrogen Burner or Lamp)
responsibility of the user of this standard to establish appro-
D3120 Test Method for Trace Quantities of Sulfur in Light
priate safety and health practices and determine the applica-
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
bility of regulatory limitations prior to use.
lometry
2. Referenced Documents
D3228 Test Method for Total Nitrogen in Lubricating Oils
and Fuel Oils by Modified Kjeldahl Method
2.1 ASTM Standards:
D3230 Test Method for Salts in Crude Oil (Electrometric
Method)
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum
D3231 Test Method for Phosphorus in Gasoline
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
D3237 Test Method for Lead in Gasoline by Atomic Ab-
Elemental Analysis.
sorption Spectroscopy
Current edition approved Feb. 15, 2010. Published March 2010. DOI: 10.1520/
D7578-10.
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 Withdrawn. The last approved version of this historical standard is referenced
the ASTM website. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7578 – 10
D3246 Test Method for Sulfur in Petroleum Gas by Oxida- D5453 Test Method for Determination of Total Sulfur in
tive Microcoulometry Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel
Engine Fuel, and Engine Oil by Ultraviolet Fluorescence
D3340 Test Method for Lithium and Sodium in Lubricating
Greases by Flame Photometer D5600 Test Method for Trace Metals in Petroleum Coke by
Inductively Coupled Plasma Atomic Emission Spectrom-
D3341 Test Method for Lead in Gasoline—Iodine
etry (ICP-AES)
Monochloride Method
D5622 Test Methods for Determination of Total Oxygen in
D3348 Test Method for Rapid Field Test for Trace Lead in
Gasoline and Methanol Fuels by Reductive Pyrolysis
Unleaded Gasoline (Colorimetric Method)
D5708 Test Methods for Determination of Nickel, Vana-
D3605 Test Method for Trace Metals in Gas Turbine Fuels
dium, and Iron in Crude Oils and Residual Fuels by
by Atomic Absorption and Flame Emission Spectroscopy
Inductively Coupled Plasma (ICP)Atomic Emission Spec-
D3831 Test Method for Manganese in Gasoline ByAtomic
trometry
Absorption Spectroscopy
D5762 Test Method for Nitrogen in Petroleum and Petro-
D4045 Test Method for Sulfur in Petroleum Products by
leum Products by Boat-Inlet Chemiluminescence
Hydrogenolysis and Rateometric Colorimetry
D5800 Test Method for Evaporation Loss of Lubricating
D4046 Test Method for Alkyl Nitrate in Diesel Fuels by
Oils by the Noack Method
Spectrophotometry
D5863 Test Methods for Determination of Nickel, Vana-
D4047 Test Method for Phosphorus in Lubricating Oils and
dium, Iron, and Sodium in Crude Oils and Residual Fuels
Additives by Quinoline Phosphomolybdate Method
by Flame Atomic Absorption Spectrometry
D4294 Test Method for Sulfur in Petroleum and Petroleum
D6334 Test Method for Sulfur in Gasoline by Wavelength
Products by Energy Dispersive X-ray Fluorescence Spec-
Dispersive X-Ray Fluorescence
trometry
D6443 Test Method for Determination of Calcium, Chlo-
D4307 Practice for Preparation of Liquid Blends for Use as
rine, Copper, Magnesium, Phosphorus, Sulfur, and Zinc in
Analytical Standards
Unused Lubricating Oils and Additives by Wavelength
D4628 Test Method for Analysis of Barium, Calcium,
Dispersive X-ray Fluorescence Spectrometry (Mathemati-
Magnesium, and Zinc in Unused Lubricating Oils by
cal Correction Procedure)
Atomic Absorption Spectrometry
D6445 Test Method for Sulfur in Gasoline by Energy-
D4629 Test Method forTrace Nitrogen in Liquid Petroleum
Dispersive X-ray Fluorescence Spectrometry
Hydrocarbons by Syringe/Inlet Oxidative Combustion and
D6470 Test Method for Salt in Crude Oils (Potentiometric
Chemiluminescence Detection
Method)
D4927 Test Methods for Elemental Analysis of Lubricant
D6481 Test Method for Determination of Phosphorus, Sul-
and Additive Components—Barium, Calcium, Phospho-
fur, Calcium, and Zinc in Lubrication Oils by Energy
rus, Sulfur, and Zinc by Wavelength-Dispersive X-Ray
Dispersive X-ray Fluorescence Spectroscopy
Fluorescence Spectroscopy
D6595 Test Method for Determination of Wear Metals and
D4929 TestMethodsforDeterminationofOrganicChloride
Contaminants in Used Lubricating Oils or Used Hydraulic
Content in Crude Oil
Fluids by Rotating Disc ElectrodeAtomic Emission Spec-
D4951 Test Method for Determination of Additive Ele-
trometry
ments in Lubricating Oils by Inductively Coupled Plasma
D6667 Test Method for Determination of Total Volatile
Atomic Emission Spectrometry
Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum
D5056 Test Method for Trace Metals in Petroleum Coke by
Gases by Ultraviolet Fluorescence
Atomic Absorption
D6728 Test Method for Determination of Contaminants in
D5059 Test Methods for Lead in Gasoline by X-Ray Spec- Gas Turbine and Diesel Engine Fuel by Rotating Disc
troscopy
Electrode Atomic Emission Spectrometry
D5184 Test Methods for Determination of Aluminum and D6732 Test Method for Determination of Copper in Jet
Silicon in Fuel Oils by Ashing, Fusion, Inductively Fuels by Graphite Furnace Atomic Absorption Spectrom-
Coupled Plasma Atomic Emission Spectrometry, and etry
Atomic Absorption Spectrometry
D6792 Practice for Quality System in Petroleum Products
and Lubricants Testing Laboratories
D5185 Test Method for Determination of Additive Ele-
ments, Wear Metals, and Contaminants in Used Lubricat-
D6920 Test Method for Total Sulfur in Naphthas, Distil-
ing Oils and Determination of Selected Elements in Base lates, Reformulated Gasolines, Diesels, Biodiesels, and
Oils by Inductively Coupled Plasma Atomic Emission
Motor Fuels by Oxidative Combustion and Electrochemi-
Spectrometry (ICP-AES) cal Detection
D5291 Test Methods for Instrumental Determination of D7039 Test Method for Sulfur in Gasoline and Diesel Fuel
Carbon, Hydrogen, and Nitrogen in Petroleum Products by Monochromatic Wavelength Dispersive X-ray Fluores-
and Lubricants cence Spectrometry
D5384 Test Methods for Chlorine in Used Petroleum Prod- D7040 Test Method for Determination of Low Levels of
ucts (Field Test Kit Method) PhosphorusinILSACGF4andSimilarGradeEngineOils
D7578 – 10
by Inductively Coupled Plasma Atomic Emission Spec- 3. Terminology
trometry
3.1 Definitions:
D7041 Test Method for Determination of Total Sulfur in
3.1.1 calibration standard, n—material with a certified
Light Hydrocarbons, Motor Fuels, and Oils by Online Gas
value for a relevant property, issued by or traceable to a
Chromatography with Flame Photometric Detection
national organization such as NIST, and whose properties are
D7111 Test Method for Determination ofTrace Elements in
known with sufficient accuracy to permit its use to evaluate the
Middle Distillate Fuels by Inductively Coupled Plasma
same property of another sample. D6792
Atomic Emission Spectrometry (ICP-AES)
3.1.2 certified reference material, CRM, n—reference ma-
D7171 Test Method for Hydrogen Content of Middle Dis-
terial one or more of whose property values are certified by a
tillate Petroleum Products by Low-Resolution Pulsed
technically valid procedure, accompanied by a traceable cer-
Nuclear Magnetic Resonance Spectroscopy
tificate or other documentation which is issued by a certifying
D7212 Test Method for Low Sulfur inAutomotive Fuels by
body. ISO Guide 30
Energy-Dispersive X-ray Fluorescence Spectrometry Us-
3.1.3 check standard, n—material having an assigned
ing a Low-Background Proportional Counter
(known) value (reference value) used to determine the accu-
D7220 Test Method for Sulfur in Automotive Fuels by
racyofthemeasurementsystemorinstrument.Thisstandardis
Polarization X-ray Fluorescence Spectrometry not used to calibrate the measurement instrument or system.
D7260 Practice for Optimization, Calibration, and Valida- D7171
tion of Inductively Coupled Plasma-Atomic Emission 3.1.4 reference material, RM, n—material with accepted
Spectrometry (ICP-AES) for ElementalAnalysis of Petro- reference value(s), accompanied by an uncertainty at a stated
leum Products and Lubricants level of confidence for desired properties, which may be used
D7303 Test Method for Determination of Metals in Lubri- for calibration or quality control purposes in the laboratory.
3.1.4.1 Discussion—Sometimes these may be prepared “in-
cating Greases by Inductively Coupled Plasma Atomic
Emission Spectrometry house” provided the reference values are established using
standard primary procedures with known precision uncertain-
D7318 Test Method for Total Inorganic Sulfate in Ethanol
ties. See below for further discussion. D6792
by Potentiometric Titration
3.1.5 traceability, n—property of the result of a measure-
D7319 Test Method for Determination of Total and Poten-
ment or the value of a standard whereby it can be related to
tial Sulfate and Inorganic Chloride in Fuel Ethanol by
stated references, usually national or international standards,
Direct Injection Suppressed Ion Chromatography
through an unbroken chain of comparisons all having stated
D7328 Test Method for Determination of Total and Poten-
uncertainties. D6792
tial Inorganic Sulfate and Total Inorganic Chloride in Fuel
Ethanol by Ion Chromatography Using Aqueous Sample
4. Summary of Guide
Injection
D7343 Practice for Optimization, Sample Handling, Cali-
4.1 Thisguidecoversproceduresusedforcalibratinginstru-
bration, and Validation of X-ray Fluorescence Spectrom- ments or methods for the analysis of petroleum products or
etry Methods for Elemental Analysis of Petroleum Prod-
lubricant samples for elemental analysis measurements. The
ucts and Lubricants means of calibration may vary from none to elaborate depen-
D7455 Practice for Sample Preparation of Petroleum and dent on the test method and the measurement technique used.
Lubricant Products for Elemental Analysis Test method requirements will take precedence over this guide
E77 Test Method for Inspection and Verification of Ther- where applicable.
4.2 This guide may also be applicable to non-petroleum
mometers
based biofuels. Work is underway to validate this.
E319 Practice for the Evaluation of Single-Pan Mechanical
Balances
5. Significance and Use
E898 Test Method of Testing Top-Loading, Direct-Reading
Laboratory Scales and Balances
5.1 Crude oil, petroleum, petroleum products, additives,
2.2 NIST Standard:
biofuels, and lubricants are routinely analyzed for their el-
emental content such as chlorine, nitrogen, hydrogen, phos-
NISTSpecial Publication 260-136 Definitions ofTerms and
phorus, sulfur, and various metals using a variety of analytical
Modes Used at NIST for Value-Assignment of Reference
techniques. Some of these methods require little to no method
Materials for Chemical Measurements
calibration; some others require only simple one step calibra-
2.3 ISO Standard:
tion; while others require elaborate calibration routine before
ISOGuide30 Termsanddefinitionsusedinconnectionwith
the product is analyzed for its elemental content.
reference materials
5.2 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
Available from National Institute of Standards and Technology (NIST), 100
practices and instructions in the test methods can be a causal
Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
factorofsucherrors.Afurtherconsequenceisanunnecessarily
Available from International Organization for Standardization (ISO), 1, ch. de
large reproducibility estimate or the data
...
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