ASTM D5827-95(2002)
(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
SIGNIFICANCE AND USE
This test method provides for the qualitative and quantitative determination of common anions in engine coolant in the milligrams per litre to low percent range and requires only a few millilitres or microlitres of sample per test, with results available in less than 30 min. Acceptable levels of chloride and other anions vary with manufacturer’blending specifications and applicable ASTM minimum or maximum specifications.
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. 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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Designation:D5827–95 (Reapproved 2002)
Standard Test Method for
Analysis of Engine Coolant for Chloride and Other Anions
by Ion Chromatography
This standard is issued under the fixed designation D5827; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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.
of the listed anions. In the case of unfamiliar formulations, Dionex AS4ASC column with AG4ASC guard columns. Other systems will require
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
sample is filtered and pumped through two ion exchange
anions of interest.
columnsandasuppressorandintoaconductivitydetector.Ions
1.4 Analysis can be performed directly by this test method
are separated based on their affinity for exchange sites of the
without pretreatment, other than dilution, as required by the
resin with respect to the resin’s affinity for the eluant. The
linear ranges of the equipment. Table 1 indicates several
suppressor increases the sensitivity of the method by both
applicable anions and approximate detection limits.
increasing the conductivity of the analytes and decreasing the
1.5 The values stated in SI units are to be regarded as the
conductivity of the eluant. The suppressor converts the eluant
standard. The values given in parentheses are for information
and the analytes to the corresponding hydrogen form acids.
only.
Anions are quantitated by integration of their response com-
1.6 This standard does not purport to address all of the
pared with an external calibration curve and are reported as
safety concerns, if any, associated with its use. It is the
milligrams per litre (mg/L).
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to its use.
4.1 This test method provides for the qualitative and quan-
titative determination of common anions in engine coolant in
2. Referenced Documents
the milligrams per litre to low percent range and requires only
2.1 ASTM Standards:
2 a few millilitres or microlitres of sample per test, with results
D1193 Specification for Reagent Water
availableinlessthan30min.Acceptablelevelsofchlorideand
D1176 Test Method for Sampling and Preparing Aqueous
other anions vary with manufacturer’s blending specifications
Solutions of Engine Coolants or Antirusts for Testing
and applicable ASTM minimum or maximum specifications.
Purposes
5. Interferences
3. Summary of Test Method
5.1 Interferences can be caused by substances with similar
3.1 A small volume of working sample is prepared by
retention times, especially if they are in high concentration
dilution of the sample with the method eluant. This diluted
compared to those of the analyte of interest. Sample dilution
will be used to minimize or solve most interference problems.
5.2 A water dip (solvent system peak) can cause interfer-
This test method is under the jurisdiction ofASTM Committee D15 on Engine
Coolants and is the direct responsibility of Subcommittee D15.04 on Chemical
ence with some integrators.This is eliminated by dilution with
Properties.
theeluantifthesampledilutionfactoris49+1(v/v)orgreater.
Current edition approved Sept. 10, 1995. Published November 1995.
2 Below this dilution, it is best to add a spike of eluant
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 15.05. concentrate to the sample such that the sample is not diluted
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5827–95 (2002)
significantly and the resulting test solution matches the eluant
used in the system. One method is the addition of 100 µL of
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.
FIG. 1 Sample Run—Chloride Peak at 1.7 min
6.4 Anion Separator Column, capable of producing analyte
separation equivalent to or better than that shown in Fig. 1.
6.5 Anion Suppressor Device—Micromembranesuppressor
ascertained that the reagent is of sufficiently high purity to
orequivalent. Acationexchangecolumninthehydrogenform
permit its use without lessening the accuracy of the determi-
has been used successfully, but it will periodically need to be
nation.
regenerated as required, being indicated by a high background
7.2 Purity of Water—Unlessotherwiseindicated,references
conductivity and low analyte response.
to water shall be understood to mean reagent water as defined
6.6 Conductivity Detector, low volume (<2 µL) and flow,
by Type II of Specification D1193. It is recommended that all
temperature compensated, capable of at least 0 to 1000 µS/cm
waterbefilteredthrougha0.2-µmfilter.Foreluantpreparation,
on a linear scale.
degas the water by sparging with helium or vacuum degassing
6.7 Integrator or Chromatography Data System Software,
and sonication.
capable of obtaining approximately the same detection limits
7.3 Eluant Buffer Stock Solution—Sodium bicarbonate
as are listed in Table 1.
(NaHCO ) 1.5 mM and sodium carbonate (Na CO ) 1.2 mM.
3 2 3
6.8 Drying Oven, controlled at 105, 150, and 600 6 5°C.
Dissolve 2.5203 6 0.0005 g of NaHCO and 2.5438 6 0.0005
6.9 Desiccator.
gofNa CO inreagentwaterina1000-mLTypeAvolumetric
2 3
flask and dilute to 1 L. Dilute 100.0 mL of this stock solution
7. Reagents
to 2000 mL in a 2-L Type A volumetric flask with degassed
7.1 Purity of Reagents—Reagent grade or higher purity
reagent water. The pH of the stock solution is 10.1 to 10.3
chemicals shall be used for the preparation of all samples,
(based on pK calculation). The eluant solution used may be
a
standards, eluants, and regenerator solutions. Unless otherwise
different if other system or analytical columns are used.
indicated, it is intended that all reagents conform to the
7.4 Stock Bromide Solution—Dry approximately2gof
specifications of the Committee onAnalytical Reagents of the
sodium bromide (NaBr) for6hat 150°C and cool in a
American Chemical Society, where such specification are
desiccator. Weigh and dissolve 1.2877 g of the dried salt in
available. Other grades may be used, provided it is first
reagent water and dilute to 1 L (1.00 mL=1.00 mg bromide).
7.5 Stock Chloride Solution—Dry approximately2gof
sodium chloride (NaCl) for1hat 600°C and cool in a
desiccator. Weigh and dissolve 1.6485 g and dilute to 1 Lwith
AnalyticalcolumnPNAS4ASCandAG4ASCguardcolumnsmanufacturedby
−
Dionex Corp., 1228 Titan Way, Sunnyvale CA 94088-3603, have been found
reagent water (1.00 mL=1.00 mg Cl ).
satisfactory for this purpose.
7.6 Stock Formate Solution—Dry approximately2gof
AMMSP.N.37106manufacturedbyDionexCorp.,1228TitanWay,Sunnyvale
sodium formate (NaHCO ) at 105°C for 6 h and cool in a
CA 94088-3603, has been found satisfactory for this purpose.
desiccator. Weigh and dissolve 1.4775 g of the salt in reagent
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
water and dilute to 1 L (1.00 mL=1.00 mg formic acid).
listed by the American Chemical Society, see Analar Standards for Laboratory
7.7 Stock Glycolic Acid Solution—Weigh and dissolve
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the U
...
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