1、Designation: D3585 08 (Reapproved 2013)Standard Specification forASTM Reference Fluid for Coolant Tests1This standard is issued under the fixed designation D3585; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. 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 specification covers a reference ethylene glycol-base test fluid to be used in providing base line data for ASTMcoolant t
3、est procedures.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility 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.
4、2. Referenced Documents2.1 ASTM Standards:2D501 Test Methods of Sampling and Chemical Analysis ofAlkaline DetergentsD538 Specification for Trisodium Phosphate (Discontinued2001) (Withdrawn 2001)3D891 Test Methods for Specific Gravity,Apparent, of LiquidIndustrial ChemicalsD1078 Test Method for Disti
5、llation Range of Volatile Or-ganic LiquidsD1119 Test Method for Percent Ash Content of EngineCoolantsD1120 Test Method for Boiling Point of Engine CoolantsD1121 Test Method for Reserve Alkalinity of Engine Cool-ants and AntirustsD1122 Test Method for Density or Relative Density ofEngine Coolant Conc
6、entrates and Engine Coolants By TheHydrometerD1123 Test Methods for Water in Engine Coolant Concen-trate by the Karl Fischer Reagent MethodD1176 Practice for Sampling and Preparing Aqueous Solu-tions of Engine Coolants or Antirusts for Testing PurposesD1177 Test Method for Freezing Point of Aqueous
7、EngineCoolantsD1287 Test Method for pH of Engine Coolants andAntirustsD1384 Test Method for Corrosion Test for Engine Coolantsin GlasswareD1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related ProductsD1881 Test Method for Foaming Ten
8、dencies of EngineCoolants in GlasswareD3634 Test Method for Trace Chloride Ion in Engine Cool-antsD5827 Test Method for Analysis of Engine Coolant forChloride and Other Anions by Ion ChromatographyD5931 Test Method for Density and Relative Density ofEngine Coolant Concentrates and Aqueous Engine Coo
9、l-ants by Digital Density MeterE202 Test Methods for Analysis of Ethylene Glycols andPropylene Glycols3. Chemical Composition Requirements3.1 The reference test fluid concentrate shall be prepared toconform to the requirements as to chemical compositionprescribed in Table 1.4. Ingredient Requirement
10、s4.1 The materials used to prepare the reference test fluidshall meet the requirements given in Annex A1 Annex A5.5. Significance and Use5.1 The data obtained for the reference test fluid areintended to be used by laboratory personnel to determine theircapability to perform tests properly. If a part
11、icular determina-tion does not fall within the prescribed limits, it has to beassumed that an error occurred in the application of the testprocedure.5.2 The coolant composition given in this specification isnot intended to be a commercial product.6. Chemical and Physical Requirements6.1 The formulat
12、ed reference test fluid concentrate shallconform to the requirements for physical and chemical prop-erties prescribed in Table 2.1This specification is under the jurisdiction ofASTM Committee D15 on EngineCoolants and Related Fluids and is the direct responsibility of SubcommitteeD15.01 on Reference
13、 Test Materials.Current edition approved Oct. 1, 2013. Published October 2013. Originallyapproved in 1989. Last previous edition approved in 2008 as D3585 08. DOI:10.1520/D3585-08R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.
14、org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-
15、2959. United States17. Performance Requirements7.1 The formulated reference test fluid concentrate shallconform to the requirements for laboratory test performanceprescribed in Table 3.8. Sampling8.1 To obtain a sample of the concentrated reference testfluid from the storage container, allow the mat
16、erial to come toroom temperature (not below 68F (20C) and shake wellbefore withdrawing the sample.8.2 All aqueous solutions to be used for test purposes shallbe prepared in accordance with Section 5 of Test MethodD1176.9. Mixing Procedure9.1 Weigh the ingredients according to the batch sizerequired.
17、9.2 Mix the ethylene and diethylene glycols.9.3 Dissolve the sodium tetraborate in the glycol mixtureusing continuous agitation.9.4 Dissolve the trisodium phosphate in the above solution.9.5 Add the sodium mercaptobenzothiazole solution andcontinue agitating the mixture until it is homogeneous.9.6 S
18、lurry the dye into a convenient portion of the solution;then add the dye slurry solution back into the formulation.9.7 Add the Pluronic L-61 antifoam and mix thoroughly.9.8 Determine the water content of the formula in accor-dance with Test Method D1123 and adjust to 4.0 6 0.2 mass %by the addition
19、of distilled water.10. Precision and Bias10.1 For statements on the precision and bias of the varioustest methods for physical and chemical properties used in thisspecification, refer to the appropriate ASTM standards.10.2 For statements on the precision and bias of the perfor-mance tests used in th
20、is specification, see the footnotes to Table3.10.3 It should be noted that the requirements listed in Table2 on physical and chemical properties, and in Table 3 onperformance, are based on the results of many differentlaboratories testing the same batch of reference test fluid.11. Packaging and Stor
21、age11.1 The test fluid concentrate may be affected by light.Therefore, after preparation, it should be packaged in opaqueplastic containers or plastic lined metal cans.11.2 Solutions prepared for testing should also be stored inopaque containers or kept in a cool, dark place to prevent theformation
22、of flocculent precipitates.11.3 Except when taking a sample, containers should beclosed to avoid absorption of moisture from the air.12. Keywords12.1 chemical composition; engine coolant; performancerequirements; specification; test fluidTABLE 1 Chemical Composition RequirementsNOTE 1The reference c
23、oolant shall be colored blue-green usingAlizarine Cyanine Green G Extra 100 % added in the proportion of 0.3 gof dye/gal of coolant.Ingredient Mass % lb/100 galAkg/m3Ethylene glycol 89.86 847.9 1016.0Diethylene glycol 5.00 47.2 56.5Sodium tetraborate, pentahydrate 3.06 28.9 34.6Trisodium phosphate,
24、dodecahydrate 0.30 2.8 3.4Sodium mercaptobenzothiazole solution(50 mass % aqueous)0.40 3.8 4.5Pluronic L-61BWaterC0.02 0.2 0.21.36 12.8 15.4ABased on a test fluid relative density of 1.133 at 60/60F (15.5/15.5C).BA nonionic polyol manufactured by BASF Corporation, 100 Cherry Hill Rd.,Parsippany, NJ
25、07054.CCalculated value; the total water content (water originally present in the basematerials, added water, water of hydration, and water of reaction and quantitativeinterference by the reaction of the reagent used (in Test Method D1123) with theingredients) should be adjusted to 4.0 0.2 mass % as
26、 the final step in thepreparation.TABLE 2 Physical and Chemical RequirementsPropertyRequirementsASTM Test Methodmin maxpH, concentrate 6.1 6.3 D128733 volume % solution 7.7 8.050 volume % solution 7.5 7.8Reserve alkalinity, mL 26.5 27.5 D1121Water content, weight % 3.8 4.2 D1123Freezing protection:
27、D1177Concentrate 23C (9F) 25C (13F)33 volume % solution 18C (0F) 19C (2F)50 volume % solution 36C (33F) 38C (36F)Relative Density at 15.6C 1.131 1.134 D1122, D5931at 20C 1.129 1.132 D891Boiling point, C (F) 330 (166) 340 (171) D1120Ash, weight % 1.4 1.6 D1119Chloride, ppm 25 D3634, D5827D3585 08 (20
28、13)2ANNEXES(Mandatory Information)A1. SPECIFICATION FOR ETHYLENE GLYCOLRequirementsProperty min max ASTM Test MethodRelative Density at 15.6/15.6C 1.115 1.118 D891A(60/60F)20/20C 1.113 1.116at (68/68F)Distillation, 760 mm, C (F) initial boiling point 88 (190) . D1078Adry point . 113 (235)Acidity (as
29、 mass % acetic acid) . 0.01 D1613AWater, mass % . 0.5 D1123Chloride, ppm . 5 D3634, D5827AThese methods are referenced in Test Methods E202.TABLE 3 Performance RequirementsATestMass Loss, max,mg/SpecimenBASTM Test MethodCorrosion in glassware D1384Copper 5Solder 5Brass 5Steel 5Cast iron 5Aluminum 15
30、Foaming volume 75 mL, maxCD1881break time 5 s, maxDAAverage data for triplicate tests.BThe multilaboratory standard deviation has been found to be 1.8 mg for all metalsthat lose an average of less than 3 mg per specimen. Therefore, results of twoproperly conducted tests from two different laboratori
31、es on samples of the same lotof reference test fluid should not differ by more than 4.1 mg, provided the averageloss is less than 3 mg per specimen. The multilaboratory standard deviation hasbeen found to be 59 % of the obtained value on metals that lose an average ofmore than 3 mg per specimen. The
32、refore, results of two properly conducted testsfrom two different laboratories on samples of the same lot of reference test fluidshould not differ by more than 167 %, provided the average loss is greater than 3mg per specimen.CThe multilaboratory standard deviation for foam volume has been found to
33、be12.0 mL. Therefore, results of two properly conducted tests from two differentlaboratories on samples of the same lot of reference test fluid should not differ bymore than 33.9 mL.DThe multilaboratory standard deviation for foam break time has been found to be0.7 s. Therefore, results of two prope
34、rly conducted tests from two differentlaboratories on samples of the same lot of reference test fluid should not differ bymore than 2.0 s.D3585 08 (2013)3A2. SPECIFICATION FOR DIETHYLENE GLYCOLProperty Requirements ASTM Test Methodmin maxRelative Density at 60/60F 1.119 1.122 D891A(15.6/15.6C)68/68F
35、 1.117 1.120at (20/20C)Distillation, 760 mm, C initial boiling point 240 (464) . D1078Adry point . 250 (482)Acidity (as mass % acetic acid) . 0.005 D1613AWater, mass % . 0.20 D1123Chloride, ppm . 5 D3634, D5827AThese methods are referenced in Test Methods E202.A3. SPECIFICATION FOR SODIUM TETRABORAT
36、E, PENTAHYDRATEAChemical AnalysisA: min maxSodium oxide (Na2O), mass % 21.3 21.7Boron trioxide (B2O3), mass % 47.8 48.7Water of crystallization, mass % 28.5 30.9Equivalent anhydrous borax (Na2B4O7), mass % 69.1 70.5Chloride . 0.05ASee Test Methods D501.A4. SPECIFICATION FOR TRISODIUM PHOSPHATE DODEC
37、AHYDRATEAChemical RequirementsA: min maxPhosphoric anhydride (P2O5), mass % 18.1 .Total alkalinity to methyl orange as Na2O, mass % 16.0 19.0Chloride . 0.1ASee Test Methods D501 and Specification D538.D3585 08 (2013)4A5. SPECIFICATION FOR SODIUM MERCAPTOBENZOTHIAZOLE SOLUTION (50 %)AChemical Require
38、mentsA: min maxSodium MBT content, mass % 49.0 51.0Free alkalinity as NaOH, mass % . 0.5Chloride, mass % . 0.1ASee Annex A6.A6. GRAVIMETRIC DETERMINATION OF SODIUM MERCAPTOBENZOTHIAZOLEA6.1 ReagentsA6.1.1 Ammonium Hydroxide (relative density 0.90)Concentrated ammonium hyroxide (NH4OH.A6.1.2 Silver N
39、itrate Solution (16 g/L) Dissolve 0.4 g ofsilver nitrate crystals in 25 mL of distilled water.A6.1.3 Hydrochloric Acid (1+1)Mix 1 volume of HCl(relative density 1.19) with 1 volume of water.A6.2 ProcedureA6.2.1 Weigh into a 250-mL beaker 0.5 to 0.6 g of thesodium mercaptobenzothiazole solution and r
40、ecord the weightto the nearest 0.1 mg.A6.2.2 Add 10 mL of concentrated ammonium hydroxide tothe beaker and dilute the contents to 150 mL with distilledwater.A6.2.3 Add the 25 mL of silver nitrate solution to theammoniacal solution while stirring.A6.2.4 Place the beaker and contents in an oven at 60C
41、 andallow the mixture to digest for 15 min.A6.2.5 Remove and allow to cool to room temperature.(The elapsed time between precipitation and the start offiltration should be a minimum of 1 h.)A6.2.6 Prepare a medium-frit Gooch crucible by placing inan oven for 15 min at 110C. Remove, place in desiccat
42、or tocool to room temperature, and then record the mass of thecrucible.A6.2.7 Filter the precipitated silver mercaptobenzothiazolethrough the fritted crucible and wash with distilled water untilno fumes of ammonia remain and the rinse liquid does not forma silver chloride precipitate with hydrochlor
43、ic acid (1 + 1).A6.2.8 Dry the crucible and precipitate to constant weightin an oven at 110C (a minimum of 2 h drying).A6.2.9 Record the weight of silver mercaptobenzothiazoleto the nearest 0.1 mg.A6.3 CalculationA6.3.1 Calculate the percentage of sodium mercaptobenzo-thiazole (NaMBT) in solution as
44、 follows:NaMBT, mass% 5 A 3189.23 3100!/B 3274.1! (A6.1)where:A = grams of dried precipitate, andB = grams of sample used.ASTM 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 expre
45、ssly advised 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
46、, either 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 a
47、ttend. 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
48、. Individual 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D3585 08 (2013)5