ASTM D3230-13 (Reaprobada 2018) Salinidad en Crudo

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: D3230 − 13 (Reapproved 2018)
Standard Test Method for

Salts in Crude Oil (Electrometric Method)1
This standard is issued under the fixed designation D3230; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope D1193 Specification for Reagent Water

1.1 This test method covers the determination of the ap- D4928 Test Method for Water in Crude Oils by Coulometric
proximate chloride (salts) concentration in crude oil. The range Karl Fischer Titration
D5002 Test Method for Density and Relative Density of
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of concentration covered is 0 mg ⁄kg to 500 mg ⁄kg or
0 lb ⁄1000 bbl to 150 lb ⁄1000 bbl as chloride concentration/ Crude Oils by Digital Density Analyzer
volume of crude oil.
3. Terminology
1.2 This test method measures conductivity in the crude oil
due to the presence of common chlorides, such as sodium, 3.1 Definitions of Terms Specific to This Standard:
calcium, and magnesium. Other conductive materials may also 3.1.1 PTB—lb/1000 bbl.
be present in the crude oil. 3.1.2 salts in crude oil—commonly, chlorides of sodium,
1.3 The values stated in SI units are to be regarded as calcium, and magnesium dissolved in crude oil. Other inor-
standard. No other units of measurement are included in this ganic chlorides may also be present.
standard.
1.3.1 Exception—Acceptable concentration units are g/m3 4. Summary of Test Method
or PTB (lb/1000 bbl).
4.1 This test method measures the conductivity of a solution
1.4 This standard does not purport to address all of the of crude oil in a mixed alcohol solvent when subjected to an
safety concerns, if any, associated with its use. It is the electrical stress. This test method measures conductivity due to
responsibility of the user of this standard to establish appro- the presence of inorganic chlorides, and other conductive
priate safety, health, and environmental practices and deter- material, in the crude oil. A homogenized test specimen is
mine the applicability of regulatory limitations prior to use. dissolved in a mixed alcohol solvent and placed in a test cell
For specific warning statements, see 7.3, 7.4, and 7.11. consisting of a beaker and a set of electrodes. A voltage is
1.5 This international standard was developed in accor- impressed on the electrodes, and the resulting current flow is
dance with internationally recognized principles on standard- measured. The chloride (salt) content is obtained by reference
ization established in the Decision on Principles for the to a calibration curve of current versus chloride concentration
Development of International Standards, Guides and Recom- of known mixtures. Calibration curves are based on standards
mendations issued by the World Trade Organization Technical prepared to approximate the type and concentration of chlo-
Barriers to Trade (TBT) Committee. rides in the crude oils being tested.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:2
D381 Test Method for Gum Content in Fuels by Jet Evapo- 5.1 This test method is used to determine the approximate
ration chloride content of crude oils, a knowledge of which is
important in deciding whether or not the crude oil needs
desalting. The efficiency of the process desalter can also be
1
This test method is under the jurisdiction of ASTM Committee D02 on evaluated.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis. 5.2 Excessive chloride left in the crude oil frequently results
Current edition approved July 1, 2018. Published August 2018. Originally in higher corrosion rates in refining units and also has
approved in 1973. Last previous edition approved in 2013 as D3230 – 13. DOI:
10.1520/D3230-13R18.
detrimental effects on catalysts used in these units.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.3 This test method provides a rapid and convenient means
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 of determining the approximate content of chlorides in crude
the ASTM website. oil and is useful to crude oil processors.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
Copyright ASTM International

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D3230 − 13 (2018)
6. Apparatus NOTE 3—Hexanes solvent is sometimes referred to or sold by other
names, such as petroleum naphtha, petroleum ether, ligroine, petroleum
6.1 The apparatus (see Annex A1) shall consist of a control benzin, and industrial naphtha. One should confirm that it meets the
unit capable of producing and displaying several voltage levels requirements of 7.4.
for applying stress to a set of electrodes suspended in a test 7.5 Calcium Chloride (CaCl2) Solution (10 g ⁄L)—Transfer
beaker containing a test solution. The apparatus shall be 1.00 g 6 0.01 g of CaCl2, or the equivalent weight of a
capable of measuring and displaying the current (mA) con- hydrated salt, into a 100 mL volumetric flask and dissolve in
ducted through the test solution between the electrodes at each 25 mL of water. Dilute to the mark with mixed alcohol solvent.
voltage level.
7.6 Magnesium Chloride (MgCl2) Solution (10 g ⁄L)—
NOTE 1—Some apparatus are capable of measuring voltage and current Transfer 1.00 g 6 0.01 g of MgCl2, or the equivalent weight of
internally and, after comparison to internal calibration curves, of display-
a hydrated salt, into 100 mL volumetric flask and dissolve in
ing the resultant concentration.
25 mL of water. Dilute to the mark with mixed alcohol solvent.
6.2 Test Beaker—See Annex A1.
7.7 Sodium Chloride (NaCl) Solution (10 g ⁄L)—Transfer
6.3 Pipet, 10 mL (total delivery), shall be used in 10.3 and 1.00 g 6 0.01 g of NaCl into a 100 mL volumetric flask and
11.1 when the viscosity of the crude oil material being dissolve in 25 mL of water. Dilute to the mark with mixed
analyzed is suitable to transfer the required volume for use in alcohol solvent.
the test (see 6.3.1). The type of pipet to use is one that is able
to be rinsed to ensure the entire volume of the material is 7.8 Oil, Refined Neutral—Any refined chloride-free oil of
contained in the intended volume. approximately 20 mm2/sec (cSt) viscosity at 40 °C and free of
6.3.1 In some cases, the viscosity of the crude oil makes it additive.
difficult and impractical to transfer 10 mL of sample using a 7.9 Salts, Mixed Solution (Concentrated Solution)—
pipet. In such cases, it is permissible to use a 10 mL graduated Combine 10.0 mL of the CaCl2 solution, 20.0 mL of the MgCl2
cylinder in place of the pipet to transfer the neutral oil (10.3) solution, and 70.0 mL of the NaCl solution, and mix thor-
and crude oil sample (11.1) to ensure consistency. The current oughly.
precision statements are based on the use of 10 mL pipets only. NOTE 4—The 10:20:70 proportions are representative of the chlorides
6.4 Cylinders, 100 mL, stoppered. present in a number of common crude oils. When the relative proportions
of calcium, magnesium, and sodium chlorides are known for a given crude
6.5 Other volumetric and graduated pipets and volumetric oil, such proportions should be used for most the accurate results.
flasks.
7.10 Salts, Mixed Solution (Dilute Solution)—Transfer 10
7. Reagents and Materials mL of the concentrated mixed chlorides solution into a
1000 mL volumetric flask, and dilute to the mark with mixed
7.1 Purity of Reagents—Reagent grade chemicals shall be
alcohol solvent.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the American 7.11 Xylene, reagent grade, minimum purity. (Warning—
Chemical Society, where such specifications are available.3 Flammable. Vapor harmful.)
Other grades may be used, provided it is first ascertained that
8. Sampling
the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination. 8.1 Obtain a sample and test specimen in accordance with
Test Method D4928. Ensure that the sample is completely
7.2 Purity of Water—Unless otherwise indicated, references
homogenized with a suitable mixer. See Test Method D4928
to water shall be understood to mean reagent water as defined
for suitable apparatus and proving.
by Type II in Specification D1193.
8.2 Samples of very viscous materials may be warmed until
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7.3 Mixed Alcohol Solvent—Mix 63 volumes of 1-butanol
they are reasonably fluid before they are sampled; however, no
and 37 volumes of absolute methyl alcohol (anhydrous). To
sample shall be heated more than is necessary to lower the
each litre of this mixture, add 3 mL of water. (Warning—
viscosity to a manageable level.
Flammable. Liquid causes eye burns. Vapor harmful. May be
fatal or cause blindness if swallowed or inhaled.) 8.3 Samples of crude oil contain water and sediment and are
inhomogeneous by nature. The presence of water and sediment
NOTE 2—The mixed alcohol solvent is suitable for use if its conduc-
tivity is less than 0.25 mA at 125 V ac (or 2 microsiemens). High will influence the conductivity of the sample. The utmost care
conductivity can be due to excess water in the solvent and can indicate that shall be taken in obtaining homogenized representative
the methyl alcohol used is not anhydrous. samples.
7.4 Hexanes, Reagent Grade, (Warning—Extremely
9. Preparation of Apparatus
flammable, harmful if inhaled.)
9.1 Support the apparatus on a level, steady surface, such as
3
a table.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not 9.2 Prepare the apparatus for operation in accordance with
listed by the American Chemical Society, see Annual Standards for Laboratory
the manufacturer’s instructions for calibrating, checking, and
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, operating the equipment. (Warning—The voltage applied to
MD. the electrodes can be as great as 250 V ac, and hazardous.)

D3230 − 13 (2018)
9.3 Thoroughly clean and dry all parts of the test beaker, the since the electronics are built-in for auto-ranging. Determination of the
electrodes, and its accessories before starting the test, being blank and the calibration standard responses are the same.
sure to remove any solvent that had been used to clean the 10.5 Repeat the procedure in 10.3, using other volumes of
apparatus. mixed salts solution (dilute solution) as needed to cover the
range of chloride contents of interest.
10. Calibration
10.6 Subtract the value obtained for the blank measurement
10.1 The conductivity of solutions is affected by the tem- from the indicated current readings of each standard sample,
perature of the specimen when measurements are made. The and plot the chloride content (ordinate) against net current
temperature of the test specimen at the time of measurement (mA) readings (abscissa) for each voltage on 3 by 3 cycle
shall be within 3 °C of the temperature at which the calibration log-log paper, or other suitable format.
curves were made.
NOTE 6—Some apparatus are capable of internally recording the current
10.2 Establish a blank measurement by following the pro- readings, standard concentration, and blank, and they provide an output in
cedure in 10.3 and 10.4, omitting the mixed salts solution. direct concentration units. Alternatively, some apparatus are also capable
When the indicated electrode current is greater than 0.25 mA at of internally converting and displaying the measured currents into
125 V ac, water or another conductive impurity is present and conductivity units of microsiemens, µS, although the precision of such
instruments was not evaluated in the 1997 interlaboratory study identified
its source must be found and eliminated before calibration can in Section 14, Precision and Bias.
be completed. Determine a blank measurement each time fresh NOTE 7—The apparatus are calibrated against standard solutions of
xylene or mixed solvent is used. neutral oil and mixed chloride solutions in xylene because of the extreme
difficulties in keeping crude oil-brine mixtures homogeneous. The cali-
10.3 Into a dry, 100 mL graduated, glass-stoppered mixing
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bration may be confirmed, if desired, by careful replicate analysis of
cylinder, add 15 mL of xylene. From a 10 mL pipet (total crude-oil samples by exhaustive extraction of salts with hot water,
delivery, see 6.3), or 10 mL graduated cylinder (see 6.3.1) followed by titration of the chlorides in the extract.
when applicable, add 10 mL of neutral oil. Rinse the 10 mL NOTE 8—In calibrating over a wide range of chloride concentrations, it
may be necessary to apply several voltages to obtain current readings
pipet or 10 mL graduated cylinder with xylene until free of oil. within the limit of the apparatus current level display (0 mA to 10 mA).
Make up to 50 mL with xylene. Stopper and shake the cylinder Higher voltages are applied for low concentrations and lower voltages are
vigorously for approximately 60 s to effect solution. Add a applied for high concentrations.
quantity of dilute mixed salts solution, in accordance with
Table 1, that is appropriate to the range of salt contents to be 11. Procedure
measured. Dilute to 100 mL with mixed alcohol solvent. Again 11.1 To a dry, 100 mL graduated, glass-stoppered cylinder,
shake the cylinder vigorously for approximately 30 s to effect add 15 mL of xylene and, using the same type of volume
solution, and allow the solution to stand approximately 5 min. transferring device used in 10.3 (that is, either a 10 mL pipet
Pour the solution into a dry test beaker. (total delivery, see 6.3), or 10 mL graduated cylinder (see
10.4 Immediately place the electrodes into the solution in 6.3.1) when applicable), transfer 10 mL of the crude oil sample
the beaker, making sure that the upper edge of the electrode into the 100 mL graduated, glass-stoppered cylinder. Rinse the
plates are below the surface of the solution. Adjust the 10 mL pipet or 10 mL graduated cylinder with xylene until free
indicated electrode voltage to a series of values, for example of oil. Make up to 50 mL with xylene. Stopper and shake the
25 V, 50 V, 125 V, 200 V, and 250 V ac. At each voltage, note cylinder vigorously for approximately 60 s. Dilute to 100 mL
the current reading and record the voltage displayed and the with mixed alcohol solvent, and again shake vigorously for
current to the nearest 0.01 mA. Remove the electrodes from the approximately 30 s. After allowing the solution to stand for
solution, rinse with xylene followed by naphtha, and allow approximately 5 min, pour it into the dry test beaker.
them to dry. 11.2 Follow the procedure in 10.4 to obtain voltage and
NOTE 5—With some apparatus, the detailed settings will not be required current readings. Record the indicated electrode current to the
nearest 0.01 mA and the nearest voltage (see Note 6).
TABLE 1 Standard Samples 11.3 Remove the electrodes from the sample solution, and
Salt, g/m 3
Salt, lb/1000 bbl Mixed Salts Solution clean the apparatus.
of Crude Oil of Crude Oil (dilute), mL
3 1.0 0.3 12. Calculation
9 3.0 1.0
15 5.0 1.5 12.1 Subtract the value obtained for the blank measurement
30 10.0 3.0 from the value obtained from the specimen measurement to
45 16.0 4.5 obtain the net current reading. From the calibration graph, read
60 21.0 6.0
75 26.0 8.0 the indicated salt concentration corresponding to the net
90 31.0 9.5 current (mA) reading of the sample (see Note 6).
115 40.0 12.0
145 51.0 15.0 12.2 Calculate the concentration in mg/kg by using the
190 66.0 20.0 appropriate equation given below:
215 75.0 22.5
245 86.00 25.5 1000X
290 101.0 30.5 Salt, mg/kg 5 (1)
d
430 151.0 45.0
Salt, mg/kg 5 2853 Y/d (2)

D3230 − 13 (2018)
where: Y = the average of two test results in lb/1000 bbl (PTB).
X = measured salt concentration in g/m3, 14.1.2 Reproducibility—The difference between two single
Y = measured salt concentration in PTB, and and independent results, obtained by different operators work-
d = specimen density at 15 C in kg/m3. ing in different laboratories on identical material, would in the
NOTE 9—The density of the specimen can be determined by various
methods, such as Test Method D5002 or other density measurement long run, exceed the following values in only one case in
methods. twenty.
R ~ mg/kg! 5 2.7803 X 0.75 (5)
13. Report
0.75
R ~ lb/1000 bbl! 5 2.069 Y (6)
13.1 Report the following information: The concentration in
mg/kg as electrometric chloride in crude oil per Test Method where:
D3230. Alternately, report the concentration directly in g/m3 or X = the average of two test results in mg/kg, and
lb/1000 bbl, if so required. Y = the average of two test results in lb/1000 bbl (PTB).
NOTE 11—Since all instruments in the 1997 interlaboratory cooperative
NOTE 10—For reporting purposes, the values stated in PTB are the
test program were calibrated in PTB and results reported in PTB, the
preferred units in the United States; in other countries, their common units
precision statement was directly obtained in PTB. The resulting precision
can be used.
data have been mathematically converted into precision in mg/kg,
14. Precision and Bias4 assuming an average density of the crude oil samples of 0.875 kg ⁄L.
14.2 Bias—The procedure in Test Method D3230 has no
14.1 Precision—The precision of this test method as deter-
bias since salt content is defined only in terms of this test
mined by the statistical examination of the 1997 interlaboratory
method and certified reference materials are unavailable.
test results is as follows:
However, since the samples from the interlaboratory study
14.1.1 Repeatability—The difference between successive
were neat desalted crudes, spiked with known quantities of salt
results, obtained by the same operator with the same apparatus
(as sea water and formation water), bias might be defined as
under constant operating conditions on identical test material,
percent recovery of halide added. Over the range from 5 g ⁄m3
would in the long run, in the normal and correct operation of
to 500 g ⁄m3 (1.5 PTB to 150 PTB) salt added, the recovery
the test method, exceed the following values in one case in
proved to be approximately constant and averaged 93 %.
twenty.
14.3 The precision statements were derived from a 1997
r ~ mg/kg! 5 0.3401 X 0.75 (3)
interlaboratory cooperative test program. Participants analyzed
0.75
r ~ lb/1000 bbl! 5 0.2531 Y (4) eight sample sets comprised of crude oils with various concen-
where: trations of chlorides. Thirteen laboratories participated with the
commercial available apparatus. See 6.3 and 6.3.1 for addi-
X = the average of two test results in mg/kg, and
tional information about the precision statements.
15. Keywords
4
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1470. Contact ASTM Customer 15.1 chlorides; crude oil; electrometric; halides; petroleum;
Service at service@astm.org. salt in crude
ANNEX
(Mandatory Information)
A1. APPARATUS
A1.1 Electrometric Chloride Apparatus (Custom Manu- A1.1.5 Transformer, plate supply 240 V, center tap, 50/60
facture) (see Fig. A1.1 and Note A1.1) Hz, 250 mA dc capacity.
A1.1.1 Milliammeter, 0 mA to 1 mA dc with 0 mA to 1 mA A1.1.6 Potentiometer, 25 Ω, ten turn.
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ac scale, 88 Ω internal resistance. A1.1.7 Potentiometer, 50 ohm, ten turn.

A1.1.2 Bridge Rectifier, full-wave, 0.75 A capacity at NOTE A1.1—An equivalent part can be substituted in each case,
60 Hz, ambient temperature; minimum of 400 PRV (Peak provided the electrical characteristics of the entire circuit remain un-
Reverse Voltage). changed and the inductive effects and stray currents are avoided.
A1.1.3 AC Voltmeter, rectifier type, 2000 Ω ⁄V, 0 V to 300 V A1.2 Test Cell Components (Custom Manufacture) (see
range. Fig. A1.2)
A1.1.4 Variable Voltage Autotransformer, input 105 V to A1.2.1 Beaker, 100 mL tall form without lip, as described
117 V, 50/60 Hz, output 0 V to 132 V, 1.75 A capacity. for use in Test Method D381.

D3230 − 13 (2018)
A1.2.2 Electrode Assembly, as shown in Fig. A1.2 and Fig. A1.4 Test Cell Components (Commercial Manufacture)
A1.3. The electrodes mounted in parallel position, exactly
A1.4.1 Beaker, 100 mL tall form without lip, as described
opposed and 6.4 mm 6 0.1 mm apart, and electrically sepa-
rated by a nylon or TFE-fluorocarbon spacer. for use in Test Method D381, is commonly used; however,
minor variations on dimensions are acceptable to accommodate
A1.3 Electrometric Chloride Apparatus (Commercial different manufacturing specifics. The beaker purpose is to
Manufacture)4 provide for containment of the specimen.
A1.3.1 The apparatus shall consist of a control unit capable A1.4.2 Electrode Assembly, shown by example in Fig. A1.2
of producing and displaying several voltage levels for applying and Fig. A1.3. The electrode assembly dimensional require-
stress to a set of electrodes suspended in a test beaker ments and means of support in the beaker are not critical to the
containing a test solution. The apparatus shall be capable of application as long as each individual component remains
measuring and displaying the current (mA) conducted through specific to the given manufactured apparatus.
the test solution between the electrodes at each voltage level
(see Note 6).
NOTE A1.2—Some apparatus is capable of measuring voltage and
current internally and after comparison to internal calibration curves,
display the resultant concentration.
A1.3.2 The actual construction specifics of the apparatus,
such as voltages utilized and means of displaying or recording
the voltage, displaying or recording the current conduction, or
calculating and displaying the calibration curves/specimen
measurements, or combination thereof, are not critical to the
application as long as each individual component remains
specific to the given manufactured apparatus (see Note 6).
FIG. A1.1 250 Volt or 540 Volt Transformer
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D3230 − 13 (2018)
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FIG. A1.2 Test Cell
FIG. A1.3 Electrode Assembly

D3230 − 13 (2018)
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

Designation: D3230 − 13 (Reapproved 2018)

Standard Test Method for

1. Scope D1193 Specification for Reagent Water

Copyright ASTM International

Copyright ASTM International

Copyright ASTM International

ac scale, 88 Ω internal resistance. A1.1.7 Potentiometer, 50 ohm, ten turn.

Copyright ASTM International

FIG. A1.1 250 Volt or 540 Volt Transformer

Copyright ASTM International

FIG. A1.2 Test Cell

FIG. A1.3 Electrode Assembly

Copyright ASTM International

Copyright ASTM International

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