1、Designation: D 3585 08Standard Specification forASTM Reference Fluid for Coolant Tests1This standard is issued under the fixed designation D 3585; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、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 test procedures.1
3、.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.2. Referenced Do
4、cuments2.1 ASTM Standards:2D 501 Test Methods of Sampling and Chemical Analysis ofAlkaline DetergentsD 538 Specification for Trisodium Phosphate (Discontinued2001)3D 891 Test Methods for Specific Gravity, Apparent, ofLiquid Industrial ChemicalsD 1078 Test Method for Distillation Range of VolatileOrg
5、anic LiquidsD 1119 Test Method for Percent Ash Content of EngineCoolantsD 1120 Test Method for Boiling Point of Engine CoolantsD 1121 Test Method for Reserve Alkalinity of EngineCoolants and AntirustsD 1122 Test Method for Density or Relative Density ofEngine Coolant Concentrates and Engine Coolants
6、 By TheHydrometerD 1123 Test Methods for Water in Engine Coolant Concen-trate by the Karl Fischer Reagent MethodD 1176 Practice for Sampling and Preparing Aqueous So-lutions of Engine Coolants or Antirusts for Testing Pur-posesD 1177 Test Method for Freezing Point of Aqueous EngineCoolantsD 1287 Tes
7、t Method for pH of Engine Coolants and Anti-rustsD 1384 Test Method for Corrosion Test for Engine Coolantsin GlasswareD 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related ProductsD 1881 Test Method for Foaming Tendencies of EngineC
8、oolants in GlasswareD 3634 Test Method for Trace Chloride Ion in EngineCoolantsD 5827 Test Method for Analysis of Engine Coolant forChloride and Other Anions by Ion ChromatographyD 5931 Test Method for Density and Relative Density ofEngine Coolant Concentrates and Aqueous Engine Cool-ants by Digital
9、 Density MeterE 202 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 Requirements4.1 The materia
10、ls 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 particular determina
11、-tion does not fall within the prescribed limits, it has to beassumed that an error occurred in the application of the testprocedure.1This specification is under the jurisdiction ofASTM Committee D15 on EngineCoolants and is the direct responsibility of Subcommittee D15.01 on Reference TestMaterials
12、.Current edition approved Oct. 1, 2008. Published November 2008. Originallyapproved in 1989. Last previous edition approved in 2002 as D 3585 98(2002).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStan
13、dards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
14、5.2 The coolant composition given in this specification isnot intended to be a commercial product.6. Chemical and Physical Requirements6.1 The formulated reference test fluid concentrate shallconform to the requirements for physical and chemical prop-erties prescribed in Table 2.7. Performance Requi
15、rements7.1 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 material to come toroom temperature (not be
16、low 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 MethodD 1176.9. Mixing Procedure9.1 Weigh the ingredients according to the batch sizerequired.9.2 Mix the ethylene and diethylene gly
17、cols.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 Slurry the dye into a convenient portion
18、 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 D 1123 and adjust to 4.0 6 0.2mass % by the addition of distilled water.TABLE 1 Chemical Co
19、mposition RequirementsNOTE 1The reference coolant 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, penta
20、hydrate 3.06 28.9 34.6Trisodium phosphate, 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 Corpo
21、ration, 100 Cherry Hill Rd.,Parsippany, NJ 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 D 1123) with theingredie
22、nts) should be adjusted to 4.0 6 0.2 mass % as the final step in thepreparation.TABLE 2 Physical and Chemical RequirementsPropertyRequirementsASTM Test Methodmin maxpH, concentrate 6.1 6.3 D 128733 volume % solution 7.7 8.050 volume % solution 7.5 7.8Reserve alkalinity, mL 26.5 27.5 D 1121Water cont
23、ent, weight % 3.8 4.2 D 1123Freezing protection: D 1177Concentrate 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 D 1122, D 5931at 20C 1.129 1.132 D 891Boiling point, C (F) 330 (166) 340 (171) D 1120Ash, weight %
24、1.4 1.6 D 1119Chloride, ppm 25 D 3634, D 5827TABLE 3 Performance RequirementsATestMass Loss, max,mg/SpecimenBASTM Test MethodCorrosion in glassware D 1384Copper 5Solder 5Brass 5Steel 5Cast iron 5Aluminum 15Foaming volume 75 mL, maxCD 1881break time 5 s, maxDAAverage data for triplicate tests.BThe mu
25、ltilaboratory standard deviation has been found to be 1.8 mg for allmetals that lose an average of less than 3 mg per specimen. Therefore, results oftwo properly conducted tests from two different laboratories on samples of thesame lot of reference test fluid should not differ by more than 4.1 mg, p
26、rovided theaverage loss is less than 3 mg per specimen. The multilaboratory standarddeviation has been found to be 59 % of the obtained value on metals that lose anaverage of more than 3 mg per specimen. Therefore, results of two properlyconducted tests from two different laboratories on samples of
27、the same lot ofreference test fluid should not differ by more than 167 %, provided the averageloss is greater than 3 mg per specimen.CThe multilaboratory standard deviation for foam volume has been found to be12.0 mL. Therefore, results of two properly conducted tests from two differentlaboratories
28、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 tobe 0.7 s. Therefore, results of two properly conducted tests from two differentlaboratories on samples of the same lot of reference te
29、st fluid should not differ bymore than 2.0 s.D358508210. 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
30、 the perfor-mance tests used in this 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
31、 test fluid.11. Packaging and Storage11.1 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, d
32、ark place to prevent theformation 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 fluidANNEXES(Mandatory Informatio
33、n)A1. SPECIFICATION FOR ETHYLENE GLYCOLRequirementsProperty min max ASTM Test MethodRelative Density at 15.6/15.6C 1.115 1.118 D 891A(60/60F)20/20C 1.113 1.116at (68/68F)Distillation, 760 mm, C (F) initial boiling point 88 (190) . D 1078Adry point . 113 (235)Acidity (as mass % acetic acid) . 0.01 D
34、1613AWater, mass % . 0.5 D 1123Chloride, ppm . 5 D 3634, D 5827AThese methods are referenced in Test Methods E 202.A2. SPECIFICATION FOR DIETHYLENE GLYCOLProperty Requirements ASTM Test Methodmin maxRelative Density at 60/60F 1.119 1.122 D 891A(15.6/15.6C)68/68F 1.117 1.120at (20/20C)Distillation, 7
35、60 mm, C initial boiling point 240 (464) . D 1078Adry point . 250 (482)Acidity (as mass % acetic acid) . 0.005 D 1613AWater, mass % . 0.20 D 1123Chloride, ppm . 5 D 3634, D 5827AThese methods are referenced in Test Methods E 202.D3585083A3. SPECIFICATION FOR SODIUM TETRABORATE, PENTAHYDRATEAChemical
36、 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 D 501.A4. SPECIFICATION FOR TRISODIUM PHOSPHATE DODECAHYDRATEAChemical Requi
37、rementsA: min maxPhosphoric anhydride (P2O5), mass % 18.1 .Total alkalinity to methyl orange as Na2O, mass % 16.0 19.0Chloride . 0.1ASee Test Methods D 501 and Specification D 538.A5. SPECIFICATION FOR SODIUM MERCAPTOBENZOTHIAZOLE SOLUTION (50 %)AChemical RequirementsA: min maxSodium MBT content, ma
38、ss % 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 Nitrate Solution (16 g/L) Dissolve 0.4
39、 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 record the weightto the nearest 0.1 mg
40、.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 andallow the mixture to digest for 1
41、5 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 desiccator tocool to room temperature, and th
42、en 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 hydrochloric acid (1 + 1).A6.2.8 Dry the crucib
43、le 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 mercaptoben-zothiazole (NaMBT) in solution as follows:NaMBT, mass % 5 A 3 189.23 3
44、 100!/B 3 274.1! (A6.1)where:A = grams of dried precipitate, andB = grams of sample used.D3585084ASTM 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 advised that determi
45、nation 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, either reapproved or wi
46、thdrawn. 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. If you feel that y
47、our 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. 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).D3585085
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