1、Designation: D 5828 97 (Reapproved 2002)Standard Test Method forCompatibility of Supplemental Coolant Additives (SCAs) andEngine Coolant Concentrates1This standard is issued under the fixed designation D 5828; the number immediately following the designation indicates the year oforiginal adoption or
2、, 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.INTRODUCTIONSupplemental coolant additives (SCAs) are used to impart special properties, u
3、sually resistance tocavitation corrosion, to engine coolants used in diesel engines with replaceable cylinder liner sleeves.Engines with this design require additives that are not normally found in commercial engine coolantconcentrates.1. Scope1.1 This test method covers determination of the compat-
4、ibility of commercial SCA and commercial ethylene andpropylene glycol engine coolant concentrates. This test methodfocuses on the solubility of specific chemical species formed inthe engine coolant. The short duration of the test (24 h), amongother restrictions, makes the test method of limited use
5、forsorting out a variety of chemical compatibility problems inwhich a component of the SCA may react with a component ofthe coolant additive package. The test as currently written alsodoes not deal with the issue of hard water compatibility, inwhich a component of the coolant or SCA additive package
6、reacts with the hardness (Ca and Mg) to form a precipitate.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is ther
7、esponsibility 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:E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Tes
8、t Method2D 1193 Specification for Reagent Water3D 1796 Test Method for Water and Sediment in Fuel Oils bythe Centrifuge Method (Laboratory Procedure)4D 3585 Specification for ASTM Reference Fluid for Cool-ant Tests53. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 engine coolant
9、 concentratean undiluted ethylene orpropylene glycol containing additives and only a small amountof water, usually less than 5 %.3.1.2 reference engine coolant concentratea standard ma-terial prepared according to the formulary given in Annex A2of this test method. This material should not be confus
10、ed withreference coolant in accordance with Specification D 3585.3.1.3 reference supplemental coolant additive (SCA)astandard SCA prepared according to the formulary given inAnnex A1 of this test method.3.1.4 supplemental coolant additivea liquid or solid ma-terial that is added to a coolant at a sp
11、ecified concentration.4. Summary of Test Method4.1 A mixture of engine coolant concentrate and deionizedwater containing approximately twice the recommended con-centration of SCA is heated to 88C (190F) for 24 h. Thesolution is centrifuged after returning to ambient temperature,and the amount of ins
12、oluble material is determined volumetri-cally and compared to the amount of insolubles obtained witha mixture of standard reference SCA and reference enginecoolant.1This test method is under the jurisdiction of ASTM Committee D15 on EngineCoolants and is the direct responsibility of Subcommittee D15
13、.11 on Heavy DutyCoolants.Current edition approved Oct. 10, 1997. Published May 1998. Originallypublished as D 5828 95.2Annual Book of ASTM Standards, Vol 14.02.3Annual Book of ASTM Standards, Vol 11.01.4Annual Book of ASTM Standards, Vol 05.01.5Annual Book of ASTM Standards, Vol 15.05.1Copyright AS
14、TM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 This test was developed to mimic the formation ofinsolubles observed in some heavy-duty diesel cooling systemsduring the mid 1980s. It measures the compatibility of SCAand
15、 coolant concentrate solutions according to their tendencyto form insolubles in service.6Such insoluble materials mayaccumulate within a cooling system, restrict heat transferthrough radiator cores, and contribute to the damage ofcomponents such as water pumps.6. Apparatus6.1 Two-pan General Laborat
16、ory Balance, 1 to 2-kg capac-ity.6.2 Centrifuge Tube, 100-mL capacity in accordance withTest Method D 1796.6.3 Centrifuge, capable of maintaining 500 rcf, with trun-nions and specimen holders suitable for the tube described in6.2.6.4 Constant Temperature Oil Bath, or equivalent, capableof maintainin
17、g the test temperature at 88C (190F), within61C (2F).6.5 Condenser Tube, glass, approximately 5-mm outsidediameter by 3-mm inside diameter by 300-mm long.6.6 Rubber Stoppers, to fit the centrifuge tube with a singlehole for the glass condenser tube.6.7 Rubber Stoppers, as above but without a hole.6.
18、8 Graduated Cylinder, 100-mL capacity to deliver.6.9 Pipette, to deliver volumes from 1 to 10 mL in 1-mLincrements.6.10 Analytical Balance, for preparing reference materialsand capable of weighing within an accuracy of 60.2 mg orbetter.7. Reagents and Materials7.1 Coolant Concentrate, and SCA for ev
19、aluation.7.2 Reference SCA, and coolant concentrate solutions (seeAnnex A1 and Annex A2).7.3 Deionized Water, in accordance with SpecificationD 1193.7.4 Nichrome Wire, or stainless steel wire.7.5 Filter Paper, Whatman No. 4 or equivalent.7.6 Plastic Containers, to store solutions. Polyethylene orpol
20、ypropylene containers with screw caps are satisfactory.8. Procedure8.1 Compatibility testing of SCA shall be conducted using aratio of 60 parts of coolant concentrate to 40 parts of awater-SCA mixture. The level of SCA in the total 60:40mixture will be approximately twice the SCA manufacturersrecomm
21、ended concentration.8.2 Fill a 100-mL centrifuge tube to the 60-mL mark withcoolant concentrate.8.3 Determine the volume of water to be added based on thephysical state and the recommended concentration of SCA tobe evaluated. Add this volume of water to the centrifuge tubeusing a graduated cylinder.
22、 For example, if the SCA is a liquidto be added at the recommended concentration of 3 % byvolume, twice the recommended concentration is 6 % or 6 mL.The volume of water to be added is 34 mL. This is 100 mL(volume of the centrifuge tube) less 60 mL (volume of coolantconcentrate required) less 6 mL (v
23、olume of SCA required).NOTE 1Using hard water will greatly influence the amount ofsolubles formed. Testing the purity of the water with a conductivity meteris recommended.NOTE 2If the SCA is a solid, prepare a sufficient volume of aconcentrated solution of the SCA in deionized water.8.4 Pipette the
24、required volume of SCA into the mixture ofcoolant concentrate and water. The sequence of mixing must beas follows: coolant concentrate, water, SCA solution. Cap witha solid rubber stopper and agitate thoroughly.NOTE 3Glycol and water mixtures exhibit a volume contraction dueto the partial molal volu
25、me effect. The final volume of the mixture shouldbe less than 100 mL, as indicated in Fig. 1.8.5 In a similar manner, add 60 mL of reference coolantconcentrate, 34 mL of deionized water, and 6 mL of referenceSCA solution to a second 100-mL centrifuge tube, and agitatethoroughly. The reference coolan
26、t must be used within 30 daysof preparation. Discard and prepare a new reference if anyinsoluble material is observed.8.6 Replace the rubber stoppers with clean air condensersprepared by inserting a 300-mm (12-in.) length of glass tubingthrough a properly sized one-hole stopper.6Hercamp and Hudgens,
27、 “Silicate Gelation in Heavy-Duty Engine CoolingSystems,” Paper No. 852327, Society of Automotive Engineers, December 1985.NOTE 1(A) nichrome wire, (B) condenser tube, and (C) immersionlevel.FIG. 1 Apparatus AssemblyD 5828 97 (2002)28.7 Insert a length of dry Nichrome or stainless steel wireinto the
28、 condenser past the bottom of the condenser tube.Immerse the centrifuge tube to the level of the solution in aconstant temperature bath at 88C (190F) for 24 h (see Fig. 1).NOTE 4The purpose of the wire is to provide a means of directingcondensate back to the centrifuge tube.8.8 At the end of the hea
29、ting period, remove the centrifugetube and solution from the bath, and cool to room temperature(allow at least 1 h). Remove the air condenser stopper, andreplace with a solid rubber stopper. Using a two-pan balance,balance the centrifuge tube, stopper, and sample against acentrifuge tube (with stopp
30、er) containing any suitable liquid.NOTE 5The centrifuge tube may be balanced against another centri-fuge tube containing another sample. A few drops of a solution of 60 %reagent grade ethylene glycol and 40 % deionized water may be added toone of the tubes to equalize the mass of the tubes.8.9 Centr
31、ifuge for 30 min at 500 rcf. Calculate the speed ofthe centrifugal rotation in r/min as follows:r/min 5 299 =rcf/r (1)where:r = radius in centimetres of the circle of rotation de-scribed by the tips of the tubes when in a rotatingposition, andrcf = 500.The following may be used as a simple means of
32、checkingthe calculation:Radius, cm (in.) r/min20.3 (8) 148025.4(10) 132536.5(12) 1210NOTE 6The following equation may be used when r is measured ininches:r/min 5 188 =rcf/r (2)NOTE 7When operating a centrifuge, tubes must be balanced properlyand used in pairs to distribute the centrifugal forces eve
33、nly.8.10 At the end of the centrifuging, stop the centrifuge andimmediately read the volume of solids in the bottom of thetube, estimating to the nearest part of a millilitre as appropriate.8.11 Clean the centrifuge tubes using the following proce-dure:8.11.1 Shake the tubes to loosen the insoluble
34、materials, anddiscard liquid and insolubles into a suitable container. Fill thetubes partially with tap water, and repeat as necessary.NOTE 8The insolubles may be loosened with the aid of an ultrasoniccleaner.8.11.2 Rinse the inside of the tubes with 1:1 HCl solution,and discard washings.8.11.3 Clea
35、n the tubes with a solution of detergent andwater, brushing as needed.8.11.4 Rinse the tubes three times with warm tap water.8.11.5 Rinse once with acetone or isopropyl alcohol toremove water, and air dry.9. Calculation and Interpretation of Results9.1 The tendency to form insolubles for the SCA-coo
36、lantconcentrate combination under evaluation is expressed inrelation to the tendency to form insolubles for the referenceSCA in a diluted reference coolant concentrate.9.2 Calculate the ratio of the volumes of insolubles formedas follows:ratio 5 A/B (3)where:A = volume of insolubles formed in the te
37、st solution, andB = volume of insolubles formed in the reference solution.10. Report10.1 Report the volume insolubles in millilitres for the testmixture, the volume insolubles in millilitres for the referencemixture, and the ratio calculated in 9.2.11. Precision and Bias11.1 PrecisionThe precision o
38、f this test method as deter-mined by an interlaboratory round robin7performed in accor-dance with Practice E 691 has been determined to be depen-dent upon the test level and may be estimated as follows:Repeatability (r) = 0.12341XReproducibility (R) = 0.31641Xwhere X = average of two results being c
39、ompared.11.1.1 In the long run, the average of two results determinedon identical materials by the same operator following thisprocedure in the same laboratory using the same equipment onthe same day will exceed the repeatability only once in twentytimes. Similarly, the average of two results determ
40、ined by twodifferent laboratories on random samples of the same batch ofidentical materials will exceed the reproducibility only once intwenty times.11.2 Table 1 shows the range of ratios determined in theround robin. The volume of insolubles measured on thereference materials was in the range from
41、0.30 to 0.80 mL.7Supporting data have been filed at ASTM Headquarters and may be obtained byrequesting RR: D 151019.TABLE 1 Range of RatiosMaterial AverageRepeatability(r)Reproducibility(R)95 Percent Limits Any Two ResultsRepeatability ReproducibilityC1:S1 0.00 0 0 0 0C1:S2 5.65 1.114 2.320 3.12 6.5
42、0C2:S1 6.52 0.803 1.916 2.25 5.36C2:S2 11.71 1.243 3.544 3.48 9.92D 5828 97 (2002)311.3 BiasNo information is available on the bias of theprocedure in this test method since the compatibility of allmaterials is determined in relation to a set of standard referencematerials.12. Keywords12.1 engine co
43、olants; supplemental coolant additives (SCA)ANNEXES(Mandatory Information)A1. PREPARATION OF REFERENCE SCA MANDATORY INFORMATIONA1.1 ComponentsAll solid components shall be certifiedACS grade chemicals, except where otherwise listed in TableA1.1. They shall be used in the proportions listed in Table
44、A1.1. Sodium hydroxide solution may be a certified high-purity reagent or prepared from ACS grade chemical andSpecification D 1193 Type IV water.A1.2 Blending Procedure:A1.2.1 Referring to Table A1.1, add Items 1, 2, and 3, mix,and heat to 66C (150F).A1.2.2 Discontinue heating when all of the sodium
45、 tetrabo-rate is dissolved (in approximately 10 to 20 min). Add Items 4and 5 (Table A1.1), and mix until all of the sodium metasilicateis dissolved.A1.2.3 Add Item 6, and mix 5 min or until dissolved.A1.2.4 Cool to ambient temperature, and filter using aWhatman No. 4 or other suitable filter medium.
46、 Store in asealed plastic container.A1.3 UsageThe recommended concentration for usageof the reference SCA is 3 % by volume. The pH of a 3 %solution of reference SCA in deionized water should be 10.5 to11.0.A2. PREPARATION OF REFERENCE COOLANT CONCENTRATEA2.1 ComponentsAll components shall be used in
47、 theproportions listed in Table A2.1. All solid components shall bereagent grade chemicals, unless otherwise indicated in TableA2.1. The ethylene glycol shall be a technical or antifreezegrade material.A2.2 Blending Procedure:A2.2.1 Referring to Table A2.1, dissolve the sodium tet-raborate pentahydr
48、ate in the ethylene glycol with stirring.A2.2.2 Add the water in a separate container, and add thesodium nitrate, sodium metasilicate pentahydrate, sodium or-thophosphate dodecahydrate, and sodium hydroxide with mildheating to assist dissolution.A2.2.3 Add the aqueous solution slowly to the glycol-b
49、oratesolution with stirring.A2.2.4 Finally add the sodium tolyltriazole solution and thePluronic L-61 solution, in that order.TABLE A1.1 ComponentsComponent Mass,%1. Water, deionized 20.002. 50 % sodium hydroxide solution 5.153. Sodium tetraborate pentahydrate (Na2B4O7,5H2O, technical grade) 10.004. Water, deionized 57.355. Sodium metasilicate pentahydrate (Na2SiO3,5H2O, technical grade) 3.506. Sodium nitrite (Na2NO2) 4.00100.00TABLE A2.1 ComponentsComponent Mass,%1. Ethylene glycol 95.782. Sodium tetraborate pentahydrate (Na2B4O75H2O, technical grade)
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