ASTM D5827-95
(Test Method)Standard Test Method for Analysis of Engine Coolant for Chloride and Other Anions by Ion Chromatography
Standard Test Method for Analysis of Engine Coolant for Chloride and Other Anions by Ion Chromatography
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for chloride ion by high-performance ion chromatography (HPIC). Several other common anions found in engine coolant can be determined in one chromatographic analysis by this test method.
1.2 This test method is applicable to both new and used engine coolant.
1.3 Coelution of other ions may cause interferences for any of the listed anions. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with the anions of interest.
1.4 Analysis can be performed directly by this test method without pretreatment, other than dilution, as required by the linear ranges of the equipment. Table 1 indicates several applicable anions and approximate detection limits.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 and health practices and determine the applicability of regulatory limitations prior to its use.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 5827 – 95
Standard Test Method for
Analysis of Engine Coolant for Chloride and Other Anions
by Ion Chromatography
This standard is issued under the fixed designation D 5827; 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.
TABLE 1 Analytes and Minimum Detection Limits
1. Scope
A
Analyte Detection Limit, mg/L
1.1 This test method covers the chemical analysis of engine
−
Chloride (Cl ) 2.0
coolant for chloride ion by high-performance ion chromatog-
−
Nitrite (NO ) 5.0
raphy (HPIC). Several other common anions found in engine
Bromide (Br) 4.0
−
coolant can be determined in one chromatographic analysis by
Nitrate (NO ) 7.1
2−
o-Phosphate (HPO ) 20.0
this test method. 4
2−
Sulfate (SO ) 8.0
1.2 This test method is applicable to both new and used
2−
Oxalate (C O ) 12.0
2 4
engine coolant.
A
Determined using 100-μL sample volume. Sample diluted 99 + 1 (v/v) with
1.3 Coelution of other ions may cause interferences for any
chromatographic eluant 30-μS/cm full scale, suppressed conductivity detection.
Dionex AS4ASC column with AG4ASC guard columns. Other systems will require
of the listed anions. In the case of unfamiliar formulations,
MDL determinations using chosen dilution factors, eluants, columns, and detector.
identification verification should be performed by either or
both fortification and dilution of the sample matrix with the
columns and a suppressor and into a conductivity detector. Ions
anions of interest.
are separated based on their affinity for exchange sites of the
1.4 Analysis can be performed directly by this test method
resin with respect to the resin’s affinity for the eluant. The
without pretreatment, other than dilution, as required by the
suppressor increases the sensitivity of the method by both
linear ranges of the equipment. Table 1 indicates several
increasing the conductivity of the analytes and decreasing the
applicable anions and approximate detection limits.
conductivity of the eluant. The suppressor converts the eluant
1.5 The values stated in SI units are to be regarded as the
and the analytes to the corresponding hydrogen form acids.
standard. The values given in parentheses are for information
Anions are quantitated by integration of their response com-
only.
pared with an external calibration curve and are reported as
1.6 This standard does not purport to address all of the
milligrams per litre (mg/L).
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
4.1 This test method provides for the qualitative and quan-
bility of regulatory limitations prior to its use.
titative determination of common anions in engine coolant in
the milligrams per litre to low percent range and requires only
2. Referenced Documents
a few millilitres or microlitres of sample per test, with results
2.1 ASTM Standards:
available in less than 30 min. Acceptable levels of chloride and
D 1193 Specification for Reagent Water
other anions vary with manufacturer’s blending specifications
D 1176 Test Method for Sampling and Preparing Aqueous
and applicable ASTM minimum or maximum specifications.
Solutions of Engine Coolants or Antirusts for Testing
Purposes
5. Interferences
5.1 Interferences can be caused by substances with similar
3. Summary of Test Method
retention times, especially if they are in high concentration
3.1 A small volume of working sample is prepared by
compared to those of the analyte of interest. Sample dilution
dilution of the sample with the method eluant. This diluted
will be used to minimize or solve most interference problems.
sample is filtered and pumped through two ion exchange
5.2 A water dip (solvent system peak) can cause interfer-
ence with some integrators. This is eliminated by dilution with
the eluant if the sample dilution factor is 49 + 1 (v/v) or greater.
This test method is under the jurisdiction of ASTM Committee D15 on Engine
Coolants and is the direct responsibility of Subcommittee D15.04 on Chemical
Below this dilution, it is best to add a spike of eluant
Properties.
concentrate to the sample such that the sample is not diluted
Current edition approved Sept. 10, 1995. Published November 1995.
2 significantly and the resulting test solution matches the eluant
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 15.05. used in the system. One method is the addition of 100 μL of
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5827
100X eluant concentrate to 10.0 mL of sample or standard.
5.3 Method interferences can be caused by the contamina-
tion of glassware, eluant, reagents, etc. Great care must be
taken to ensure that contamination, especially by chloride, is
kept at the lowest possible levels.
5.4 Pre-rinsing of the sample preparation containers with
deionized water is mandatory.
5.5 The use of latex gloves is highly recommended to
prevent contamination.
6. Apparatus
6.1 Analytical Balance, capable of weighing accurately to
0.0001 g.
6.2 Ion Chromatograph—Analytical system with all re-
quired accessories including syringes, columns, suppressor,
gasses, and detector. Column life and performance are en-
hanced by the use of a two-eluant channel gradient pump, if
available.
6.3 Guard Column, for protection of the analytical column
from strongly retained constituents. Better separations are
obtained with additional plates.
6.4 Anion Separator Column, capable of producing analyte
separation equivalent to or better than that shown in Fig. 1.
FIG. 1 Sample Run—Chloride Peak at 1.7 min
6.5 Anion Suppressor Device—Micro membrane suppressor
or equivalent. A cation exchange column in the hydrogen form
7.2 Purity of Water—Unless otherwise indicated, references
has been used successfully, but it will periodically need to be
to water shall be understood to mean reagent water as defined
regenerated as required, being indicated by a high background
by Type II of Specification D 1193. It is recommended that all
conductivity and low analyte response.
water be filtered through a 0.2-μm filter. For eluant preparation,
6.6 Conductivity Detector, low volume (<2 μL) and flow,
degas the water by sparging with helium or vacuum degassing
temperature compensated, capable of at least 0 to 1000 μS/cm
and sonication.
on a linear scale.
7.3 Eluant Buffer Stock Solution—Sodium bicarbonate
6.7 Integrator or Chromatography Data System Software,
(NaHCO ) 1.5 mM and sodium carbonate (Na CO ) 1.2 mM.
capable of obtaining approximately the same detection limits 3 2 3
Dissolve 2.5203 6 0.0005 g of NaHCO and 2.5438 6 0.0005
as are listed in Table 1. 3
gofNa CO in reagent water in a 1000-mL Type A volumetric
6.8 Drying Oven, controlled at 105, 150, and 600 6 5°C. 2 3
flask and dilute to 1 L. Dilute 100.0 mL of this stock solution
6.9 Desiccator.
to 2000 mL in a 2-L Type A volumetric flask with degassed
7. Reagents
reagent water. The pH of the stock solution is 10.1 to 10.3
(based on pK calculation). The eluant solution used may be
a
7.1 Purity of Reagents—Reagent grade or higher purity
different if other system or analytical columns are used.
chemicals shall be used for the preparation of all samples,
7.4 Stock Bromide Solution—Dry approximately2gof
standards, eluants, and regenerator solutions. Unless otherwise
sodium bromide (NaBr) for6hat 150°C and cool in a
indicated, it is intended that all reagents conform to the
desiccator. Weigh and dissolve 1.2877 g of the dried salt in
specifications of the Committee on Analytical Reagents of the
reagent water and dilute to 1 L (1.00 mL = 1.00 mg bromide).
American Chemical Society, where such specification are
7.5 Stock Chloride Solution—Dry approximately2gof
available. Other grades may be used, provided it is first
sodium chloride (NaCl) for1hat 600°C and cool in a
ascertained that the reagent is of sufficiently high purity to
desiccator. Weigh and dissolve 1.6485 g and dilute to 1 L with
permit its use without lessening the accuracy of the determi-
−
reagent water (1.00 mL = 1.00 mg Cl ).
nation.
7.6 Stock Formate Solution—Dry approximately2gof
sodium formate (NaHCO ) at 105°C for 6 h and cool in a
desiccator. Weigh and dissolve 1.4775 g of the salt in reagent
Analytical column PN AS4ASC and AG4ASC guard columns manufactured by
Dionex Corp., 1228 Titan Way, Sunnyvale CA 94088-3603, have been found water and dilute to 1 L (1.00 mL = 1.00 mg formic acid).
satisfactory for this purpose.
7.7 Stock Glycolic Acid Solution—Weigh and dissolve
AMMS P.N. 37106 manufactured by Dionex Corp., 1228 Titan Way, Sunnyvale
1.0000 g of the solid acid in reagent water and dilute to 1 L
CA 94088-3603, has been found satisfactory for this purpose.
(1.00 mL = 1.00 mg glycolate).
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
7.8 Stock Nitrate Solution—Dry approximately2gofso-
listed by the American Chemical Society, see Analar Standards for Laboratory
dium nitrate (NaNO ) for 24 h at 105°C and cool in a
Chemicals, BDH Ltd., Poole, Dorset, U.K.,
...
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