1、Designation: D 6130 97a (Reapproved 2003)Standard Test Method forDetermination of Silicon and Other Elements in EngineCoolant by Inductively Coupled Plasma-Atomic EmissionSpectroscopy1This standard is issued under the fixed designation D 6130; the number immediately following the designation indicat
2、es the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of
3、 silicon inengine coolant by inductively coupled plasma-atomic emissionspectroscopy (ICP-AES). Silicon can be determined as low asthe range of 5 ppm by this test method. Other elements alsofound in engine coolant can be determined by this method.This test method is applicable to the determination of
4、 dissolvedor dispersed elements.1.2 This test method is applicable to both new and usedengine coolant.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility
5、of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2D 1176 Standard Practice for Sampling and PreparingAqueous Solut
6、ions of Engine Coolants or Antirusts forTesting Purposes3E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method42.2 US EPA Standards:Method 6010, Inductively Coupled Plasma Method, SW-846, Test Methods for Evaluating Solid Waste5Method 200.7, Inductively Co
7、upled Plasma - Atomic Emis-sion Spectrometric Method for Trace Element Analysis ofWater And Wastes, EPA-600/4-79-020, revised 198453. Summary of Test Method3.1 Elements in solution are determined, either sequentiallyor simultaneously, by ICP-AES. New or used engine coolantsare prepared by dilution.
8、Samples and standards are introducedto the nebulizer using a peristaltic pump and the aerosol isinjected into an argon-supported inductively coupled plasma.The high temperature of the plasma atomizes the sample andproduces atomic emission intensities at wavelengths associatedwith the desired element
9、s. Emission intensity is proportional toconcentration. Elemental determinations are made by compar-ing standard and sample emission intensities.4. Significance and Use4.1 Some engine coolants are formulated with silicon con-taining additives. This test method provides a means ofdetermining the conce
10、ntration of dissolved or dispersed ele-ments which give an indication of this additive content in theengine coolant.5. Interferences5.1 Interferences may be categorized as follows:5.1.1 SpectralLight emission from spectral sources otherthan the element of interest may contribute to apparent netsigna
11、l intensity. Sources of spectral interference include directspectral line overlaps, broadened wings of intense spectrallines, ion-atom recombination continuum emission, molecularband emission and stray (scattered) light from the emission ofelements at high concentrations. Avoid overlaps by selecting
12、alternate analytical wavelengths.5.1.2 PhysicalPhysical interferences are effects associ-ated with sample nebulization and transport processes such asviscosity and particulate contamination.5.1.3 BackgroundHigh background effects from scatteredlight, etc., can be compensated for by background correc
13、tionadjacent to the analyte line.5.1.4 ChemicalChemical interferences are caused by mo-lecular compound formation, ionization effects, and thermo-chemical effects associated with sample vaporization andatomization in the plasma. Normally these effects are not1This test method is under the jurisdicti
14、on of ASTM Committee D15 on EngineCoolants and is the direct responsibility of Subcommittee D15.04 on ChemicalProperties.Current edition approved Oct. 10, 1997. Published July 1998. Originallypublished as D 613097. Last previous edition D 613097.2Annual Book of ASTM Standards, Vol 11.01.3Annual Book
15、 of ASTM Standards, Vol 15.05.4Annual Book of ASTM Standards, Vol 14.02.5Available from U. S. Environmental Protection Agency, Environmental Moni-toring and Support Laboratory, Cincinnati, OH 45268.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, U
16、nited States.pronounced and can be minimized by careful selection ofoperating conditions (incident power, plasma observation po-sition, etc.).6. Apparatus6.1 SpectrometerAn inductively coupled plasma emissionspectrometer of the simultaneous or sequential type includingRF generator, torch, nebulizer,
17、 spray chamber, recommendedperistaltic pump and host computer.7. Reagents and Materials7.1 Purity of ChemicalsReagent grade or better chemicalsshall be used for preparation of all standards and samples.Other grades may be used provided it is first ascertained thatthe reagent is of sufficiently high
18、purity to permit its usewithout lessening the accuracy of the determination.7.2 Purity of WaterReferences to water shall be under-stood to mean deionized water.7.3 Standard Stock SolutionsCertified solutions may bepurchased or prepared from high purity grade chemicals ormetals (See Method 6010, SW-8
19、46, Method 200.7). Standardscontain 1000 mg/L of the element of interest. Salts should bedried as indicated.7.4 Calibration StandardsPrepare the standards in volu-metric flasks using appropriate volumes of each stock solutionto cover the expected concentration range of the samples.Elements in multie
20、lement standards should be shown to becompatible and stable. Compensate for differences in standard/sample matrix by using an appropriate amount of ethyleneglycol and/or an internal standard. Suggested combinations andanalytical lines are in Table 1. Validate calibration standards.Monitor stability.
21、8. Sampling8.1 Collect sample in accordance with Practice D 1176.9. Calibration and Standardization9.1 Set the up instrument according to the manufacturersinstructions. Warm it up at least 20 min.9.2 Profile and calibrate the instrument according to manu-facturers recommended procedures with the bla
22、nk and stan-dards, aspirating the standard for at least 30 s to allow theinstrument to equilibrate prior to signal integration. Watershould be run for an additional 60 s after standards containingboron. Calibration should be validated and stability of stan-dards should be monitored.10. Sample Prepar
23、ation10.1 Dilute the sample with deionized water so the concen-tration of the element(s) of interest is in the linear detectionrange of the instrument. Generally a120 or150 dilution for usedengine coolant and a1100 dilution for engine coolant concen-trate are sufficient. Samples may be prepared by w
24、eight tovolume or by volume to volume. Be certain when preparingdilutions by volume that the entire sample aliquot is trans-ferred. Filter or centrifuge samples that contain particulate.11. Procedure11.1 Aspirate the prepared samples into the calibratedinstrument using the same conditions establishe
25、d for thecalibration procedure. Rinse sufficiently to prevent carryover.Run water an additional 60 s between samples containingboron.11.2 Run a blank and an instrument check standard (acalibration standard, calibration verification or standard enginecoolant) every ten samples or as established to be
26、 necessary forthe instrument. Analyze a blank and check standard at the endof each run. The concentration shall be within 65 % of theexpected value. If the concentration is out of range, correct theproblem, recalibrate the instrument and rerun the samples inquestion.11.3 Matrix spikes and duplicates
27、 may be performed asquality control procedures if sample concentrations are suspectdue to contamination, spectral interferences or trace levels ofthe element of interest.11.4 Perform the corrections and calculations, includingdilution factors, using the instrument host computer.12. Report12.1 Sample
28、s prepared by weight to volume dilution may bereported in ppm by weight or % by weight depending on theconcentration of the element of interest. Samples prepared byvolume may be reported as g/L, mg/L, g/mL, etc. These unitsmay be converted to ppm weight or % by weight using thedensity of the sample:
29、concentration ppm by wt!5concentration g/mL!density g/mL!(1)13. Precision and Bias13.1 PrecisionThe precision of this test method for sili-con was determined by statistical examination of interlabora-tory results according to Practice E 691 is as follows:613.1.1 RepeatabilityThe difference between s
30、uccessivetest results obtained by the same operator on the same testmaterial would, in the long run, in the normal and correctoperation of the test method, be expected to be as indicated inTable 2. Average relative repeatability, that is, within labora-tory consistency, is 6 %.6Supporting data are a
31、vailable from ASTM Headquarters. Request RR:D151013.TABLE 1 Analytical Wavelengths for ICP-AES Determination ofElements in Engine CoolantElement Wavelength, nmMixed Standard 1Silicon 251.612, 288.158, 252.851, 252.411Molybdenum 202.030, 204.598Boron 249.773Phosphorus 214.914, 178.29Mixed Standard 2A
32、luminum 308.215, 394.401, 369.152Lead 220.353Zinc 213.856Iron 259.94, 259.837, 238.204Copper 324.754, 219.226Magnesium 279.079, 280.270, 279.553Calcium 317.933, 393.37, 396.847, 315.887Sodium 588.995, 589.592D 6130 97a (2003)213.1.2 ReproducibilityThe difference between two singleand independent res
33、ults, obtained by different operators work-ing in different laboratories on identical test materials would, inthe long run, in the normal and correct operation of this testmethod, be expected to be as indicated in Table 2. The relativereproducibility never exceeds twice the repeatability and onavera
34、ge is about 1-12 times, at 9 %, the repeatability.NOTE 1Ten laboratories and six samples were involved in thisinterlaboratory study. Data from only seven laboratories are available.13.2 BiasSince there is no accepted reference materialsuitable for determining the bias for this test method, bias hasn
35、ot been determined.14. Keywords14.1 engine coolant; inductively coupled plasma-atomicemission spectroscopy; siliconASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly ad
36、vised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, eithe
37、r reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend.
38、If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Indiv
39、idual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).TABLE 2 Summary of Precision ParametersRepeatability ReproducibilitySample Average, Absolute, Relative, % Absolute, Relative, %g/mL g/mL g/mLB 246 20.6 8 27.4 11D 250 16.1 6 28.1 11A 513 28.0 5 55.7 11F 515 28.0 5 35.5 7C 645 26.4 4 48.6 8E 649 36.4 6 53.0 8D 6130 97a (2003)3
