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 Most test methods spell out the calibration requirements but often do not quote the frequency required letting the laboratories use good laboratory practices for this task.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.

1. 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.

2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

ASTM Standards

D129 Test Method for Sulfur in Petroleum Products (General High Pressure Decomposition Device Method)

D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)

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

D892 Test Method for Foaming Characteristics of Lubricating Oils

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)

D1548 Test Method for Vanadium in Heavy Fuel Oil1

D1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)

D1839 Test Method for Amyl Nitrate in Diesel Fuels

D2622 Test Method for Sulfur in Petroleum Products by Wavelength Dispersive X-ray Fluorescence Spectrometry

D2784 Test Method for Sulfur in Liquefied Petroleum Gases (Oxy-Hydrogen Burner or Lamp)

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

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

D3831 Test Method for Manganese in Gasoline By Atomic Absorption Spectroscopy

D4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry

D4046 Test Method for Alkyl Nitrate in Diesel Fuels by Spectrophotometry

D4047 Test Method for Phosphorus in Lubricating Oils and Additives by Quinoline Phosphomolybdate Method

D4294 Test Method for Sulfur in Petroleum and Petroleum Products by Energy Dispersive X-ray Fluorescence Spectrometry

D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards

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 Petroleum Hydrocarbons by Syringe/Inlet Oxidative Combustion and Chemiluminescence Detection

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 Methods 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 Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and Determination of Selected Elements in 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 Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence

D5800 Test Method for Evaporation Loss of Lubricating Oils by the Noack Method

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

D6470 Test Method for Salt in Crude Oils (Potentiometric Method)

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

D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories

D6920 Test Method for Total Sulfur in Naphthas, Distillates, Reformulated Gasolines, Diesels, Biodiesels, and Motor Fuels by Oxidative Combustion and Electrochemical Detection

D7039 Test Method for Sulfur in Gasoline and Diesel Fuel 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 Light Hydrocarbons, Motor Fuels, and Oils by Online 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 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

D7455 Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis

E77 Test Method for Inspection and Verification of Thermometers

E319 Practice for the Evaluation of Single-Pan Mechanical Balances

E898 Test Method of Testing Top-Loading, Direct-Reading Laboratory Scales and Balances

NIST Standard

ISO Standard

Keywords

atomic absorption spectrometry; balances; calibration; calibration standard; check standard; electrometric methods; ICP-AES methods; lubricants; petroleum products; photometric methods; reference material; temperature measuring devices; timers; verification; XRF methods;

ICS Code

ICS Number Code 75.080 (Petroleum products in general); 75.100 (Lubricants, industrial oils and related products)

DOI: 10.1520/D7578-10E01

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ASTM D7578