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ASTM D5762-98

(Test Method)

Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence

Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence

SCOPE
1.1 This test method covers the determination of nitrogen in liquid hydrocarbons, including petroleum process streams and lubricating oils in the concentration range from 40 to 10 000 μg/g nitrogen. For light hydrocarbons containing less than 100 μg/g nitrogen, Test Method D 4629 can be more appropriate.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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. Specific hazard statements are given in Section 6, 7.1, 8.2, and 8.2.2.

General Information

Status
Historical
Publication Date
09-Apr-2002
ICS
75.040 - Crude petroleum
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Replaced By
ASTM D5762-01 - Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence
Effective Date
10-Apr-2002

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ASTM D5762-98 - Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet ChemiluminescenceASTM D5762-98 - Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence
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ASTM D5762-98 - Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence
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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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: D 5762 – 98 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Nitrogen in Petroleum and Petroleum Products by Boat-Inlet
1
Chemiluminescence
This standard is issued under the fixed designation D 5762; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This test method covers the determination of nitrogen in 4.1 Many nitrogen compounds can contaminate refinery
liquid hydrocarbons, including petroleum process streams and catalysts. They tend to be the most difficult class of compounds
lubricating oils in the concentration range from 40 to 10 000 to hydrogenate, so the nitrogen content remaining in the
μg/g nitrogen. For light hydrocarbons containing less than 100 product of a hydrotreator is a measure of the effectiveness of
μg/g nitrogen, Test Method D 4629 can be more appropriate. the hydrotreating process. In lubricating oils the concentration
1.2 The values stated in SI units are to be regarded as the of nitrogen is a measure of the presence of nitrogen containing
standard. The values given in parentheses are for information additives. This test method is intended for use in plant control
only. and in research.
1.3 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 Boat Inlet System, capable of being sealed to the inlet of
the combustion tube and swept with inert gas. The boats are
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. fabricated from platinum or quartz. To aid quantitative liquid
injection, add a small piece of quartz wool to the boat. The boat
2. Referenced Documents
drive mechanism should be able to fully insert the boat into the
2.1 ASTM Standards: furnace tube inlet section. A drive mechanism that advances
D 4052 Test Method for Density and Relative Density of and withdraws the sample boat into and out of the furnace at a
2
Liquids by Digital Density Meter controlled and repeatable rate is required.
D 4057 Practice for Manual Sampling of Petroleum and 5.2 Chemiluminescence Detector, capable of measuring
2
Petroleum Products light emitted from the reaction between nitric oxide and ozone,
D 4177 Practice for Automatic Sampling of Petroleum and and containing a variable attenuation amplifier, integrator, and
2
Petroleum Products readout.
D 4629 Test Method for Trace Nitrogen in Liquid Petro- 5.3 Combustion Tube, fabricated from quartz. The inlet end
leum Hydrocarbons by Syringe/Inlet Oxidative Combus- of the tube shall be large enough to accept the sample boat and
2
tion and Chemiluminescence Detection to have side arms for introduction of oxygen and inert gas. The
construction is such that the carrier gases sweep the inlet zone
3. Summary of Test Method
transporting all of the volatilized sample into a high-
3.1 A hydrocarbon sample is placed on a sample boat at
temperature oxidation zone. The oxidation section should be
room temperature. The sample and boat are advanced into a large enough to ensure complete oxidation of the sample.
high-temperature combustion tube where the nitrogen is oxi-
Combustion tubes recommended for the two furnaces in 5.5.1
dized to nitric oxide (NO) in an oxygen atmosphere. The NO and 5.5.2 are described in 5.3.1 and 5.3.2. Other configurations
contacts ozone and is converted to excited nitrogen dioxide
are acceptable if precision and bias are not degraded.
(NO ). The light emitted as the excited NO decays is detected 5.3.1 Quartz combustion tube for use with the single-zone
2 2
by a photomultiplier tube, and the resulting signal is a measure
furnace is illustrated in Fig. 1. A water-jacket around the inlet
of the nitrogen contained in the sample. section can be used to cool the boat prior to sample injection.
5.3.2 Quartz combustion tube for use with the two-zone
furnace is illustrated in Fig. 2. Fig. 3 illustrates a combustion
1
tube for a two-zone furnace that is equipped with the ability to
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee switch to a pure oxygen carrier gas flow after the boat has been
D02.03 on Elemental Analysis.
fully extended into the furnace (consult the instrument manual
Current edition approved Dec. 10, 1998. Published Februar
...

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1.3 This test method is limited to the use of X-ray fluorescence (XRF) spectrometers employing an X-ray tube for excitation in conjunction with wavelength dispersive detection system or energy dispersive high resolution semiconductor detector with the ability to separate signals of adjacent and near-adjacent elements.  
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Note 1: Defined as having a Reid vapor pressure less than 82.7 kPa (12 psi).  
1.2 This test method details procedures for the production of a liquefied gas, distillate fractions, and residuum of standardized quality on which analytical data can be obtained, and the determination of yields of the above fractions by both mass and volume. From the preceding information, a graph of temperature versus mass % distilled can be produced. This distillation curve corresponds to a laboratory technique, which is defined at 15/5 (15 theoretical plate column, 5:1 reflux ratio) or TBP (true boiling point).  
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4.1 Theoretically, all of the sediment and water determination methods are valid for crude oils containing from 0 % to 100 % by volume sediment and water; the range of application is specified within the scope of each method. The round robins for all methods were conducted on relatively dry oil. All precision and bias statements included in the methods are based upon the round robin data. Analysis becomes more challenging with crude oils containing higher water contents due to the difficulty in obtaining a representative sample, and maintaining the sample quality until analysis begins.  
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5.1 This test method describes a sensitive method for estimating the intrinsic stability of an oil. The intrinsic stability is expressed as S-value. An oil with a low S-value is likely to undergo flocculation of asphaltenes when stressed (for example, extended heated storage) or blended with a range of other oils. Two oils each with a high S-value are likely to maintain asphaltenes in a peptized state and not lead to asphaltene flocculation when blended together.  
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1.1 This test method covers procedures for quantifying the intrinsic stability of the asphaltenes in an oil by automatic instruments using optical detection.  
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5.1 Crude oils and oil sands bitumen contain naturally occurring acidic species. Acidity of crude oil has been implicated in corrosion of distribution and process systems. The relative amount of these materials can be determined by titrating with bases. The acid number is a measure of this amount of acidic substance in the oil under the conditions of the test.  
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1.1 This test method covers the determination of acidic components in crude oil and petroleum products including waxes, bitumen, base stocks, and asphalts that are soluble in mixtures of xylenes and propan-2-ol. It is applicable for the determination of acids whose dissociation constants in water are larger than 10–9; extremely weak acids whose dissociation constants are smaller than 10–9 do not interfere. The values obtained by this test method may not be numerically equivalent to other acid value measurements. The range of KOH acid numbers included in the precision statement is 0.1 mg/g to 16 mg/g.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D5863-22(Test Method)
Standard Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame Atomic Absorption Spectrometry

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5.1 When fuels are combusted, metals present in the fuels can form low melting compounds that are corrosive to metal parts. Metals present at trace levels in petroleum can deactivate catalysts during processing. These test methods provide a means of quantitatively determining the concentrations of vanadium, nickel, iron, and sodium. Thus, these test methods can be used to aid in determining the quality and value of the crude oil and residual oil.
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1.1 These test methods cover the determination of nickel, vanadium, iron, and sodium in crude oils and residual fuels by flame atomic absorption spectrometry (AAS). Two different test methods are presented.  
1.2 Procedure A, Sections 8–14—Flame AAS is used to analyze a sample that is decomposed with acid for the determination of total Ni, V, and Fe.  
1.3 Procedure B, Sections 15–20—Flame AAS is used to analyze a sample diluted with an organic solvent for the determination of Ni, V, and Na. This test method uses oil-soluble metals for calibration to determine dissolved metals and does not purport to quantitatively determine nor detect insoluble particulates. Hence, this test method may underestimate the metal content, especially sodium, present as inorganic sodium salts.  
1.4 The concentration ranges covered by these test methods are determined by the sensitivity of the instruments, the amount of sample taken for analysis, and the dilution volume. A specific statement is given in Note 1.  
1.5 For each element, each test method has its own unique precision. The user can select the appropriate test method based on the precision required for the specific analysis.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard, unless specifically stated. Other units that appear in this standard are included for information purposes only or because they are in embedded pictures that cannot be edited.  
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. Specific warning statements are given in 8.1, 9.2, 9.5, 11.2, 11.4, and 16.1.  
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1.3 This test method may be used for the determination of cut point carbon fraction intervals (see 3.2.1) of live crude oils and condensates from initial boiling point (IBP) to 391 °C (nC24). The nC24 plus fraction is reported.  
1.4 Dead oils or condensates sampled in accordance with 12.1 may also be analyzed.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5.1 Exception—Where there is no direct SI equivalent such as tubing size.  
1.6 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.  
1.7 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.

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5.1 Insoluble material may form in oils that are subjected to oxidizing conditions.  
5.2 Significant formation of oil insolubles or metal corrosion products, or both, during this test may indicate that the oil will form insolubles or corrode metals, or both, during field service. However, no correlation with field service has been established.
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1.1 This test method covers and is used to evaluate the tendency of inhibited mineral oil based steam turbine lubricants and mineral oil based anti-wear hydraulic oils to corrode copper catalyst metal and to form sludge during oxidation in the presence of oxygen, water, and copper and iron metals at an elevated temperature. The test method is also used for testing circulating oils having a specific gravity less than that of water and containing rust and oxidation inhibitors.  
Note 1: During round robin testing copper and iron in the oil, water and sludge phases were measured. However, the values for the total iron were found to be so low (that is, below 0.8 mg), that statistical analysis was inappropriate. The results of the cooperative test program are available (see Section 16).  
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1.3 Procedure A of this test method requires the determination and report of the weight of the sludge and the total amount of copper in the oil, water, and sludge phases. Procedure B requires the sludge determination only. The acid number determination is optional for both procedures.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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1.7 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.

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Standard Test Method for Determination of Organic Chloride Content in Crude Oil

SIGNIFICANCE AND USE
5.1 Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.  
5.1.1 Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.
5.1.1.1 Most trade contracts specify that no organic chloride is present in the crude oil.  
5.1.2 Several pipelines have set specification limits at  
5.1.2.1 To ensure Eq 3).  
5.1.3 Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and are destroyed during hydro-treating (desulfurization of the naphtha).  
5.2 Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on the refining operations as the organic chlorides.  
5.3 Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and the acid accumulates in condensing regions of the refinery. Unexpected concentrations of organic chlorides cannot be effectively neutralized and damage can result. Organic chlorides are not known to be naturally present in crude oils and usually result from cleaning operations at producing sites, pipelines, or tanks. It is important for the oil industry to have common methods available for the determination of organic chlorides in crude oil, particularly when transfer of custody is involved.
SCOPE
1.1 The procedures in this test method cover the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using either distillation and sodium biphenyl reduction, distillation and microcoulometry, or distillation and X-ray fluorescence (XRF) spectrometry.  
1.2 The procedures in this test method involve the distillation of crude oil test specimens to obtain a naphtha fraction prior to chloride determination. The chloride content of the naphtha fraction of the whole crude oil can thereby be obtained. See Section 6 regarding potential interferences.  
1.3 Procedure A covers the determination of organic chloride in the washed naphtha fraction of crude oil by sodium biphenyl reduction followed by potentiometric titration.  
1.4 Procedure B covers the determination of organic chloride in the washed naphtha fraction of crude oil by oxidative combustion followed by microcoulometric titration.  
1.5 Procedure C covers the determination of organic chloride in the washed naphtha fraction of crude oil by X-ray fluorescence spectrometry.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentration units are micrograms of chloride per gram of sample, though milligrams of chloride per kilogram of sample is commonly used for Procedure C.  
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.

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