1、Designation: D 3585 98 (Reapproved 2002)Standard 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 r
2、evision. 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 specification covers a reference ethylene glycol-base test fluid to be used in providing base line data for ASTMcoolan
3、t test 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 u
4、se.2. Referenced Documents2.1 ASTM Standards:D 501 Test Methods of Sampling and Chemical Analysis ofAlkaline Detergents2D 538 Specification for Trisodium Phosphate2D 891 Test Methods for Specific Gravity, Apparent, ofLiquid Industrial Chemicals3D 1078 Test Method for Distillation Range of VolatileOr
5、ganic Liquids4D 1119 Test Method for Ash Content of Engine Coolantsand Antirusts3D 1120 Test Method for Boiling Point of Engine Coolants3D 1121 Test Method for Reserve Alkalinity of EngineCoolant and Antirusts3D 1122 Test Method for Density or Relative Density ofEngine Coolant Concentrates and Engin
6、e Coolants by theHydrometer3D 1123 Test Method for Water in Engine Coolant Concen-trate by the Karl Fischer Reagent Method3D 1176 Test Method for Sampling and Preparing AqueousSolutions of Engine Coolants or Antirusts for TestingPurposes3D 1177 Test Method for Freezing Point of Aqueous EngineCoolant
7、s3D 1287 Test Method for pH of Engine Coolants and Anti-rusts3D 1384 Test Method for Corrosion Test for Engine Coolantsin Glassware3D 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related Products4D 1881 Test Method for Foaming Tenden
8、cies of EngineCoolants in Glassware3D 3634 Test Method for Trace Chloride Ion in EngineCoolants3D 5827 Test Method for Analysis of Engine Coolant forChloride and Other Anions by Ion Chromatography3D 5931 Test Method for Density and Relative Density ofEngine Coolant Concentrates and Aqueous Engine Co
9、ol-ants by Digital Density Meter3E 202 Test Methods for Analysis of Ethylene Glycols andPropylene Glycols33. 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 Require
10、ments4.1 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
11、particular 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 form
12、ulated reference test fluid concentrate shallconform to the requirements for physical and chemical prop-erties prescribed in Table 2.1This specification is under the jurisdiction of ASTM Committee D15 on EngineCoolants and is the direct responsibility of Subcommittee D15.01 on Reference TestMaterial
13、s.Current edition approved April 10, 1998. Published December 1998. Originallypublished as D 3583 89. Last previous edition D 3585 95.2Annual Book of ASTM Standards, Vol 15.04.3Annual Book of ASTM Standards, Vol 15.05.4Annual Book of ASTM Standards, Vol 06.03.1Copyright ASTM International, 100 Barr
14、Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. 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 refere
15、nce testfluid from the storage container, allow the material 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 MethodD 1176.9. Mixing Procedure9.1 We
16、igh the ingredients according to the batch sizerequired.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 andcont
17、inue agitating the mixture until it is homogeneous.9.6 Slurry the dye into a convenient portion of the solution;then add the dye slurry to 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 a
18、djust to 4.0 6 0.2mass % by the addition 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
19、bias of 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 re
20、ference 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
21、cool, dark 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 fluidTABLE 1 Chemical Comp
22、osition 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, pentahy
23、drate 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 Corpora
24、tion, 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 (in Test Method D 1123) with theingredients) sh
25、ould be adjusted to 4.0 6 0.2 mass % as the final step in thepreparation.D 35852ANNEXES(Mandatory Information)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,
26、C (F) initial boiling point 88 . D 1078Adry point . 113Acidity (as mass % acetic acid) . 0.01 D 1613AWater, mass % . 0.5 D 1123TABLE 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 7.8Re
27、serve alkalinity, mL 26.5 27.5 D 1121Water content, weight % 3.8 4.2 D 1123Freezing protection: D 1177Concentrate 23C (10F) 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
28、, C (F) 330 (166) 340 (171) D 1120Ash, weight % 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
29、, maxDAAverage data for triplicate tests.BThe multilaboratory 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 tes
30、t fluid should not differ by more than 4.1 mg, provided 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 test
31、s from two different laboratories on samples of 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
32、 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 tobe 0.7 s. Therefore, results of two properly conducted tests from two differentlaborat
33、ories on samples of the same lot of reference test fluid should not differ bymore than 2.0 s.D 35853RequirementsProperty min max ASTM Test MethodChloride, ppm . 5 D 3634, D 5827AThese methods are referenced in Test Methods E 202.A2. SPECIFICATION FOR DIETHYLENE GLYCOLProperty Requirements ASTM Test
34、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, 760 mm, C initial boiling point 240 . D 1078Adry point . 250Acidity (as mass % acetic acid) . 0.005 D 1613AWater, mass % . 0.20 D 1123Chloride, ppm . 5 D 3634, D 5827AThese methods are re
35、ferenced in Test Methods E 202.A3. SPECIFICATION FOR SODIUM TETRABORATE, 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 . 0.05
36、ASee Test Methods D 501.A4. SPECIFICATION FOR TRISODIUM PHOSPHATE DODECAHYDRATEAChemical RequirementsA: 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 SODI
37、UM MERCAPTOBENZOTHIAZOLE SOLUTION (50 %)AChemical RequirementsA: 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
38、.90)Concentrated ammonium hyroxide (NH4OH.A6.1.2 Silver Nitrate 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 t
39、o 0.6 g of thesodium mercaptobenzothiazole solution and record 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.D 35854A6.2.3 Add the 25 mL of silver nitrate solution to theammoniacal solution while
40、 stirring.A6.2.4 Place the beaker and contents in an oven at 60C 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
41、 placing inan oven for 15 min at 110C. Remove, place in desiccator 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 l
42、iquid does not forma silver chloride precipitate with hydrochloric 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 pe
43、rcentage of sodium mercaptoben-zothiazole (NaMBT) in solution as follows:NaMBT, mass % 5 A 3 189.23 3 100!/B 3 274.1! (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
44、any item mentionedin this standard. Users of this standard are expressly 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 technic
45、al committee and must be reviewed every five years andif not revised, 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
46、 at a meeting of theresponsible technical committee, which you may attend. 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 Harbo
47、r 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).D 35855
