ASTM D6470-99(2015)
(Test Method)Standard Test Method for Salt in Crude Oils (Potentiometric Method)
Standard Test Method for Salt in Crude Oils (Potentiometric Method)
SIGNIFICANCE AND USE
4.1 A knowledge of water extractable inorganic halides in oil is important when deciding whether or not the oils need desalting. Excessive halide, especially in crude oil, frequently results in higher corrosion rates in refining units.
SCOPE
1.1 This test method covers the determination of salt in crude oils. For the purpose of this test method, salt is expressed as % (m/m) NaCl (sodium chloride) and covers the range from 0.0005 % to 0.15 % (m/m).
1.2 The limit of detection is 0.0002 % (m/m) for salt (as NaCl).
1.3 The test method is applicable to nearly all of the heavier petroleum products, such as crude oils, residues, and fuel oils. It may also be applied to used turbine oil and marine diesel fuel to estimate seawater contamination. Water extractable salts, originating from additives present in oils, are codetermined.
1.4 The values stated in SI units are to be regarded as the standard.
1.5 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.
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Designation: D6470 − 99 (Reapproved 2015)
Standard Test Method for
1
Salt in Crude Oils (Potentiometric Method)
This standard is issued under the fixed designation D6470; 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 D4928 Test Method for Water in Crude Oils by Coulometric
Karl Fischer Titration
1.1 This test method covers the determination of salt in
E200 Practice for Preparation, Standardization, and Storage
crudeoils.Forthepurposeofthistestmethod,saltisexpressed
of Standard and Reagent Solutions for ChemicalAnalysis
as % (m/m) NaCl (sodium chloride) and covers the range from
0.0005 % to 0.15 % (m/m).
3. Summary of Test Method
1.2 The limit of detection is 0.0002 % (m/m) for salt (as
3.1 After homogenizing the crude oil with a mixer, a
NaCl).
weighed aliquot is dissolved in xylene at 65 °C and extracted
1.3 The test method is applicable to nearly all of the heavier
with specified volumes of alcohol, acetone, and water in an
petroleum products, such as crude oils, residues, and fuel oils.
electrically heated extraction apparatus. A portion of the
Itmayalsobeappliedtousedturbineoilandmarinedieselfuel
aqueous extract is analyzed for total halides by potentiometric
to estimate seawater contamination. Water extractable salts,
titration.
originating from additives present in oils, are codetermined.
1.4 The values stated in SI units are to be regarded as the
4. Significance and Use
standard.
4.1 A knowledge of water extractable inorganic halides in
1.5 This standard does not purport to address all of the
oil is important when deciding whether or not the oils need
safety concerns, if any, associated with its use. It is the
desalting. Excessive halide, especially in crude oil, frequently
responsibility of the user of this standard to establish appro-
results in higher corrosion rates in refining units.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Apparatus
5.1 Extraction Apparatus, made of borosilicate glass, con-
2. Referenced Documents
formingtothedimensionsgiveninFig.1,andconsistingofthe
2
2.1 ASTM Standards:
following component parts:
D329 Specification for Acetone
5.1.1 Boiling Flask, 500 mL capacity.
D770 Specification for Isopropyl Alcohol
5.1.2 Hopkins Reflux Condenser, having a vapor outlet
D843 Specification for Nitration Grade Xylene
connected by a rubber tube to an outside vent or to a suction
D1193 Specification for Reagent Water
hood.
D4006 Test Method for Water in Crude Oil by Distillation
5.1.3 Thistle Tube, approximately 70 mL capacity, with a
D4057 Practice for Manual Sampling of Petroleum and
line to indicate approximately the 50 mL level.
Petroleum Products
5.1.4 Heating Tube, containing a chimney for increasing
D4177 Practice for Automatic Sampling of Petroleum and
convection in the liquid.
Petroleum Products
5.1.5 Heating Coil, 250 W, consisting of a suitable gage of
D4377 Test Method forWater in Crude Oils by Potentiomet-
Nichrome wire.
ric Karl Fischer Titration
5.1.6 Rheostat, of suitable resistance and capacity, for
regulating the heater.
1
This test method is under the jurisdiction of ASTM Committee D02 on
5.2 Safety Shield, colorless safety glass, or equivalent, to be
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
mounted in front of the extraction apparatus (see 5.1).
Current edition approved April 1, 2015. Published May 2015. Originally
5.3 Sampling Tube, glass, length approximately 600 mm,
approved in 1999. Last previous edition approved in 2010 as D6470 – 99 (2010).
DOI: 10.1520/D6470-99R15.
I.D. approximately 5 mm, with a bulb having a volume of
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
100 mL, or more, and drawn out at one end to an opening of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
inside diameter (I.D.) 2 mm to 3 mm.Apipette with cut-off tip
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. makes a suitable sample tube.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6470 − 99 (2015)
NOTE 1—Hopkins-type condenser is used.
FIG. 1 Extraction Apparatus
5.4 Potentiometric Titration Equipment, with a measuring 6. Reagents and Materials
accuracy of 62 mV, or better, provided with a silver indicating
6.1 Purity of Reagents—Unless otherwise indicated, it is
and a glass reference electrode and
...
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: D6470 − 99 (Reapproved 2010) D6470 − 99 (Reapproved 2015)
Standard Test Method for
1
Salt in Crude Oils (Potentiometric Method)
This standard is issued under the fixed designation D6470; 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 test method covers the determination of salt in crude oils. For the purpose of this test method, salt is expressed as %
(m/m) NaCl (sodium chloride) and covers the range from 0.00050.0005 % to 0.15 % (m/m).
1.2 The limit of detection is 0.0002 % (m/m) for salt (as NaCl).
1.3 The test method is applicable to nearly all of the heavier petroleum products, such as crude oils, residues, and fuel oils. It
may also be applied to used turbine oil and marine diesel fuel to estimate seawater contamination. Water extractable salts,
originating from additives present in oils, are codetermined.
1.4 The values stated in SI units are to be regarded as the standard.
1.5 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
2
2.1 ASTM Standards:
D329 Specification for Acetone
D770 Specification for Isopropyl Alcohol
D843 Specification for Nitration Grade Xylene
D1193 Specification for Reagent Water
D4006 Test Method for Water in Crude Oil by Distillation
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4377 Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration
D4928 Test Method for Water in Crude Oils by Coulometric Karl Fischer Titration
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
3. Summary of Test Method
3.1 After homogenizing the crude oil with a mixer, a weighed aliquot is dissolved in xylene at 65°C65 °C and extracted with
specified volumes of alcohol, acetone, and water in an electrically heated extraction apparatus. A portion of the aqueous extract
is analyzed for total halides by potentiometric titration.
4. Significance and Use
4.1 A knowledge of water extractable inorganic halides in oil is important when deciding whether or not the oils need desalting.
Excessive halide, especially in crude oil, frequently results in higher corrosion rates in refining units.
5. Apparatus
5.1 Extraction Apparatus, made of borosilicate glass, conforming to the dimensions given in Fig. 1, and consisting of the
following component parts:
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved May 1, 2010April 1, 2015. Published May 20102015. Originally approved in 1999. Last previous edition approved in 20042010 as
D6470D6470 – 99 (2010).–99 (2004). DOI: 10.1520/D6470-99R10.10.1520/D6470-99R15.
2
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6470 − 99 (2015)
NOTE 1—Hopkins-type condenser is used.
FIG. 1 Extraction Apparatus
5.1.1 Boiling Flask, 500 mL 500 mL capacity.
5.1.2 Hopkins Reflux Condenser, having a vapor outlet connected by a rubber tube to an outside vent or to a suction hood.
5.1.3 Thistle Tube, approximately 70 mL 70 mL capacity, with a line to indicate approximately the 50 mL 50 mL level.
5.1.4 Heating Tube, containing a chimney for increasing convection in the liquid.
5.1.5 Heating Coil, 250 W, 250 W, consisting of a suitable gage of Nichrome wire.
5.1.6 Rheostat, of suitable resistance and capacity, for regulating the heater.
5.2 Safety Shield, colorless safety glass, or equivalent, to be mounted in front of the extraction apparatus (see 5.1).
5.3 Sampling Tube, glass, length approximately 600 mm, 600 mm, I.
...
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