1、Designation: D6130 11 (Reapproved 2018)Standard Test Method forDetermination of Silicon and Other Elements in EngineCoolant by Inductively Coupled Plasma-Atomic EmissionSpectroscopy1This standard is issued under the fixed designation D6130; the number immediately following the designation indicates
2、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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of sil
3、icon 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 dis
4、solvedor 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 asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if an
5、y, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internation
6、ally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Speci
7、fication for Reagent WaterD1176 Practice for Sampling and Preparing Aqueous Solu-tions of Engine Coolants or Antirusts for Testing PurposesE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Tes
8、t Method2.2 U.S. EPA Standards:3Method 6010, Inductively Coupled Plasma Method, SW-846, Test Methods for Evaluating Solid WasteMethod 200.7, Inductively Coupled Plasma - Atomic Emis-sion Spectrometric Method for Trace Element Analysis ofWater And Wastes, EPA-600/4-79-020, revised 19843. Summary of T
9、est Method3.1 Elements in solution are determined, either sequentiallyor simultaneously, by ICP-AES. New or used engine coolantsare prepared by dilution. Samples and standards are introducedto the nebulizer using a peristaltic pump and the aerosol isinjected into an argon-supported inductively coupl
10、ed plasma.The high temperature of the plasma atomizes the sample andproduces atomic emission intensities at wavelengths associatedwith the desired elements. Emission intensity is proportional toconcentration. Elemental determinations are made by compar-ing standard and sample emission intensities.4.
11、 Significance and Use4.1 Some engine coolants are formulated with silicon con-taining additives. This test method provides a means ofdetermining the concentration of dissolved or dispersed ele-ments which give an indication of this additive content in theengine coolant.5. Interferences5.1 Interferen
12、ces may be categorized as follows:5.1.1 SpectralLight emission from spectral sources otherthan the element of interest may contribute to apparent netsignal intensity. Sources of spectral interference include directspectral line overlaps, broadened wings of intense spectrallines, ion-atom recombinati
13、on continuum emission, molecularband emission and stray (scattered) light from the emission of1This test method is under the jurisdiction of ASTM Committee D15 on EngineCoolants and Related Fluids and is the direct responsibility of SubcommitteeD15.04 on Chemical Properties.Current edition approved
14、March 1, 2018. Published March 2018. Originallyapproved in 1997. Last previous edition approved in 2011 as D613011. DOI:10.1520/D6130-11R18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volum
15、e information, refer to the standards Document Summary page onthe ASTM website.3Available from U.S. Environmental Protection Agency, Environmental Moni-toring and Support Laboratory, Cincinnati, OH 45268.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29
16、59. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical
17、Barriers to Trade (TBT) Committee.1elements at high concentrations. Avoid overlaps by selectingalternate analytical wavelengths.5.1.2 PhysicalPhysical interferences are effects associatedwith sample nebulization and transport processes such asviscosity and particulate contamination.5.1.3 BackgroundH
18、igh background effects from scatteredlight, etc., can be compensated for by background correctionadjacent 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 andatomi
19、zation in the plasma. Normally these effects are notpronounced and can be minimized by careful selection ofoperating conditions (incident power, plasma observationposition, etc.).6. Apparatus6.1 SpectrometerAn inductively coupled plasma emissionspectrometer of the simultaneous or sequential type inc
20、ludingRF generator, torch, nebulizer, 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 tha
21、tthe reagent is of sufficiently high 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 chem
22、icals ormetals (See Method 6010, SW-846, 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 ra
23、nge of the samples.Elements in multielement 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 cal
24、ibration standards.Monitor stability.8. Sampling8.1 Collect sample in accordance with Practice D1176.9. 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
25、 recommended procedures with the blank andstandards, 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 sho
26、uld be monitored.10. Sample Preparation10.1 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 suffic
27、ient. Samples may be prepared by weight 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 us
28、ing the same conditions established 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 t
29、en samples or as established to be 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
30、.11.3 Matrix spikes and duplicates 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 h
31、ost computer.12. Report12.1 Samples 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 weig
32、ht using thedensity of the sample: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 2Aluminum 308.215, 3
33、94.401, 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, 589.592D6130 11 (2018)2concentration ppm by wt! 5concentration g/mL!density g/mL!(1)13. Precision and Bias413.1 The p
34、recision of this test method is based on aninterlaboratory study conducted in 2009. A total of ninelaboratories participated in this study, testing samples of sixdifferent coolants for their metals content. Every test resultrepresents an individual determination, and all participantswere asked to re
35、port four replicate test results for eachmetal/coolant combination. Practice E691 was followed for thedesign and analysis of the data; the details are given inRR:D15-1030.13.1.1 Repeatability Limit, rTwo test results obtainedwithin one laboratory shall be judged not equivalent if theydiffer by more
36、than the r value for that material; r is the intervalrepresenting the critical difference between two test results forthe same material, obtained by the same operator using thesame equipment on the same day in the same laboratory.13.1.1.1 Repeatability limits are listed in Tables 2-13.13.1.2 Reprodu
37、cibility limit, RTwo test results shall bejudged not equivalent if they differ by more than the R valuefor that material; R is the interval representing the criticaldifference between two test results for the same material,obtained by different operators using different equipment indifferent laborat
38、ories.13.1.2.1 Reproducibility limits are listed in Tables 2-13.13.1.3 The above terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E177.13.1.4 Any judgment in accordance with statements 13.1.1and 13.1.2 would have an approximate 95% probability ofbeing correct.
39、13.2 BiasAt the time of the study, there was no acceptedreference material suitable for determining the bias for this testmethod, therefore no statement on bias is being made.13.3 The precision statement was determined through sta-tistical examination of 1,872 test results, submitted by ninelaborato
40、ries, on twelve metals, in six coolants.13.3.1 The six coolant types were described as follows:Coolant ACoolant BCoolant CCoolant DCoolant ECoolant F13.4 To judge the equivalency of two test results, it isrecommended to choose the coolant material that is closest incharacteristics to the test materi
41、al.14. Keywords14.1 engine coolant; inductively coupled plasma-atomicemission spectroscopy; silicon4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting RR:D15-1030.TABLE 2 Aluminum (g/mL)MaterialAverage,ARepeatabilityStandardDeviation, SrReproducibilit
42、yStandardDeviation, SRRepeatabilityLimit, rReproducibilityLimit, RSample A 6.4 8.0 9.7 22.4 27.2Sample B 2.9 3.0 3.2 8.3 9.0Sample C 0.5 0.7 0.7 2.0 2.1Sample D 2.9 4.4 4.9 12.4 13.9Sample E 5.2 3.7 4.8 10.2 13.5Sample F 5.6 6.1 7.0 17.2 19.7AThe average of the laboratories calculated averages.D6130
43、 11 (2018)3TABLE 3 Boron (g/mL)MaterialAverage,ARepeatabilityStandardDeviation, SrReproducibilityStandardDeviation, SRRepeatabilityLimit, rReproducibilityLimit, RSample A 215.8 5.3 29.3 14.7 82.1Sample B 193.5 169.5 222.7 474.6 623.5Sample C 298.8 98.2 131.6 274.8 368.5Sample D 388.8 334.9 447.3 937
44、.6 1252.5Sample E 139.3 123.7 161.1 346.2 451.1Sample F 91.8 78.2 103.2 218.9 288.9AThe average of the laboratories calculated averages.TABLE 4 Calcium (g/mL)MaterialAverage,ARepeatabilityStandardDeviation, SrReproducibilityStandardDeviation, SRRepeatabilityLimit, rReproducibilityLimit, RSample A 3.
45、9 4.2 5.1 11.6 14.2Sample B 7.0 1.2 2.1 3.5 5.9Sample C 9.0 5.2 6.5 14.6 18.1Sample D 12.6 5.3 5.8 15.0 16.3Sample E 3.6 0.7 0.8 2.1 2.3Sample F 3.7 2.3 3.0 6.5 8.5AThe average of the laboratories calculated averages.TABLE 5 Copper (g/mL)MaterialAverage,ARepeatabilityStandardDeviation, SrReproducibi
46、lityStandardDeviation, SRRepeatabilityLimit, rReproducibilityLimit, RSample A 1.4 1.6 1.8 4.4 5.1Sample B 5.0 1.3 1.6 3.8 4.4Sample C 4.8 3.8 5.0 10.7 13.9Sample D 2.9 1.3 1.8 3.6 4.9Sample E 4.1 3.5 3.9 9.7 11.0Sample F 2.6 2.5 3.4 7.1 9.6AThe average of the laboratories calculated averages.TABLE 6
47、 Iron (g/mL)MaterialAverage,ARepeatabilityStandardDeviation, SrReproducibilityStandardDeviation, SRRepeatabilityLimit, rReproducibilityLimit, RSample A 7.3 0.7 4.7 2.1 13.1Sample B 41.0 34.5 45.8 96.5 128.2Sample C 2.3 2.1 2.6 6.0 7.4Sample D 23.5 7.1 10.2 20.0 28.5Sample E 1.9 2.9 3.0 8.0 8.5Sample
48、 F 4.9 4.3 6.2 11.9 17.3AThe average of the laboratories calculated averages.D6130 11 (2018)4TABLE 7 Lead (g/mL)MaterialAverage,ARepeatabilityStandardDeviation, SrReproducibilityStandardDeviation, SRRepeatabilityLimit, rReproducibilityLimit, RSample A 2.8 3.0 4.2 8.4 11.6Sample B 1.8 1.7 2.2 4.8 6.1
49、Sample C 4.9 2.8 3.2 7.8 9.1Sample D 3.2 1.7 2.5 4.7 7.1Sample E 5.5 5.0 5.6 14.0 15.6Sample F 3.3 3.1 4.9 8.7 13.7AThe average of the laboratories calculated averages.TABLE 8 Magnesium (g/mL)MaterialAverage,ARepeatabilityStandardDeviation, SrReproducibilityStandardDeviation, SRRepeatabilityLimit, rReproducibilityLimit, RSample A 3.4 3.7 4.6 10.2 13.0Sample B 3.0 2.1 2.4 5.9 6.9Sample C 2.4 1.6 2.1 4.5 5.8Sample D 2.2 1.7 2.0 4.6 5.7Sample E 1.6 1.4 1.7 3.8 4.6Sample F 2.9 2.5 4.0 7.0 11.3AThe average of the lab
