1、Designation: D3342 90 (Reapproved 2017)Standard Test Method forDispersion Stability of New (Unused) Rolling OilDispersions in Water1This standard is issued under the fixed designation D3342; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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 determination of the dispersionstability of dispersions of rolling oils in
3、 water. It is applicableto oils whose water dispersions are stable under moderateagitation, but which show at least some separation uponstanding quiescent for12 h, by rising of the oil particles.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are includ
4、ed in thisstandard.1.3 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
5、use. For specificwarning statements, see 6.2, A2.1, and A2.5.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendation
6、s issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1126 Test Method for Hardness in WaterD1293 Test Methods for pH of Water3. Summary of Test Method3.1 The rolling oil is dispersed in a standard test water, in astandard con
7、tainer, under standard conditions of time,agitation, and concentration. When the agitation is stopped, theresulting decrease in oil concentration at a specified point nearthe bottom of the container is measured at certain time intervalsand plotted.4. Significance and Use4.1 Each steel rolling mill a
8、nd operation is particular as tothe degree of stability of dispersion required to effect maxi-mum efficiency of lubrication and cooling. This test method isdesigned to differentiate between coolants for this use. Asimilar situation is encountered with aluminum rolling mills,but significant differenc
9、es in designated settling times berequired outside the parameter of times used herein. Precisiondata have only been obtained relative to metastable dispersionsfor steel mill rolling oils.5. Apparatus5.1 Mixing Beaker,3,45800 mL capacity, made of stainlesssteel, modified as shown in Annex A2.5.2 Comb
10、ination Agitator and Temperature ControlDevice.4,55.3 Babcock Centrifuge Bottles4,6The 165 mm cream testbottle, with 5 mL-neck permitting oil concentration readingsfrom 0 % to 10 % is preferred. These bottles should be markedfor filling to the 50 mL level which will normally be foundclose to the jun
11、ction of body and neck. Sulfonation bottles mayalso be used.5.4 Centrifuge, capable of whirling the Babcock bottles atsufficient speed to give a clean separation of oil and waterunder the test conditions. A centrifuge giving a relativecentrifugal force (rcf) of 5009 at the bottle tips has been found
12、to give good separations in 10 min.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.L0.04 on Metal Deformation Fluids and Lubricants.Current edition approved June 1, 2017. Publishe
13、d July 2017. Originally approvedin 1990. Last previous edition approved in 2012 as D3342 90 (2012).DOI:10.1520/D3342-90R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, re
14、fer to the standards Document Summary page onthe ASTM website.3The sole source of supply of the apparatus (beaker #2-584F) known to thecommittee at this time is Fisher Scientific.4If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comme
15、nts will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.5The sole source of supply of the apparatus (the Porta-temp) known to thecommittee at this time is Precision Scientific Co.6The sole source of supply of the apparatus (cream test bottle
16、No. 12-705 orsulfonation bottle No. 6-904) known to the committee at this time is FisherScientific.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized
17、principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.5 To calculate the rpm required to achieve the stated rcf,use the fo
18、llowing formula:rpm 5 1335=rcf/d (1)where:rcf = relative centrifugal force,d = diameter of swing measured between tips of oppositetubes when in rotating position, mm, andrpm = revolutions per minute.5.6 Stop Watch, or similar timing device.6. Reagents6.1 Buffered Synthetic Hard Water, prepared in ac
19、cordancewith Annex A2.6.2 Sulfuric Acid, 30 % by volume in water. Lower acidconcentrations may be used if clean separations are obtained.(WarningSulfuric acid is poison, corrosive, and a strongoxidizer.)7. Procedure7.1 The flow rate of the combination agitator and tempera-ture control device should
20、be between 3500 mL min and4500 mL min. The flow rate should be measured with a pieceof 6.35 mm inside diameter bore plastic tubing temporarilyattached to the pump outlet and removed after this measure-ment. During the test, do not use attachments such as tubing,stopcocks, pinch clamps, etc. on the p
21、ump outlet.7.2 Add 4275 mL of test water to the beaker, install theagitator-temperature control device, and adjust it for 60 Ctemperature. When the water reaches this temperature, add225 mL of the rolling oil to be tested. (The oil sample shouldbe sufficiently agitated to assure complete mixing of o
22、ilcomponents. With most materials, sufficient heat to melt all ofthe components will also be required, however, at no timeshould the temperature exceed 60 C.) Continue controlledtemperature agitation for 30 min.7.3 While agitation continues, fill one Babcock bottle for anemulsion concentration contr
23、ol test, as follows: Open the pinchclamp on the beaker sample tap for 2 s to 3 s. Discard about20 mL of emulsion to flush the tap, and attempt to come ascleanly as possible to the end. Close the pinch clamp, place thehose tip in a Babcock bottle, and fill it at a rapid flow rate to the50 mL mark.7.4
24、 Stop agitation and restart the stop watch at zero time.Fill Babcock bottles as described above at 30 s and 1 min,2 min, 4 min, 8 min, 16 min, and 32 min elapsed time. It ispermissible to stop sampling sooner or later (such as at 16 minor 64 min) if such data are desired, but earlier sample timesmay
25、 not be omitted even for very stable emulsions, because thesampling process slightly affects further settling rates. For eachsample, purge the sample tap several seconds ahead of time sothat filling the Babcock bottle starts at the correct time.7.5 Fill each Babcock bottle to the upper graduation li
26、newith 30 % by volume sulfuric acid. Swirl while filling. Spin inthe centrifuge for 10 min, or until a clean separation isobtained. It may be necessary to use a different mineral acid orto heat the filled Babcock bottles to facilitate a clean separa-tion. (If however, none of these methods results i
27、n a cleanseparation, the test method cannot be considered applicable forthat particular oil.) Read the difference in levels in terms of theBabcock bottle calibration scale at the top and bottom of the oillayer.8. Calculation8.1 For the sample bottle taken as a control during agitation,calculate the
28、percent of oil found. Since the calibrations on theneck of the Babcock bottle usually range from 0 to 50, andcorrespond to 10 % oil in this test method, the difference inscale reading between the top and bottom of the oil layerdivided by 5 equals the percent oil. If this result is not close to5 %, t
29、he results are suspect until repeat runs verify thereproducibility of the discrepancy. Significant amounts ofwater soluble compounds in the oil sample might explain lowconcentrations, for example. If, by the end of the 30 minagitation period, any significant amount of free oil or invertedemulsion re
30、mains floating on the surface without being repeat-edly drawn down into the water layer, the oil is probably toodifficult to disperse for the test method to be applicable.8.2 For each sample taken after agitation was stopped,calculate the amount of oil found as a percent of the amountfound in the sa
31、mple.8.3 A single number used to describe the rolling oil emul-sion stability is the slope of a straight line, fit by the method ofleast squares, to the base ten logarithms of both time, inminutes, and the measured concentrations in percent. Inpractice, to avoid taking the of zero, use the concentra
32、tion plus1%.8.4 The estimate of the Slope b, for an experimental trial iseasily obtained by completing the following worksheet.Log10TimeLog10Concentration+1%Time Actual Coded (X) (Y) XY0.5 0.30103 0.903091.0 0.0 0.602062.0 0.30103 0.301034.0 0.60206 0.08.0 0.90309 0.3010316.0 1.20412 0.6020632.0 1.5
33、0515 0.903098.5 Enter the log of the test result plus 1 on the appropriateline. Form the product of each coded time (X) and thecorresponding concentration (Y). Add the seven resultingvalues. The slope is then calculated by the following formula:b 5(XY/2.53733 (2)9. Report9.1 The test result should b
34、e reported by the form in Fig. 1,or equivalent. Calculations of Slope b (see 8.4) are to be usedto test the precision of test method and define the stability ofthe dispersion by a single number.D3342 90 (2017)210. Precision and Bias10.1 Precision7The precision of the test method as ob-tained by stat
35、istical examination of interlaboratory test resultsis as follows:10.1.1 RepeatabilityThe difference between successivetest results, obtained by the same operator with the sameapparatus under constant operating conditions on identical testmaterial, would in the long run, in the normal and correctoper
36、ation of the test method, exceed the following value onlyin one case in twenty:0.0736 slope10.1.2 ReproducibilityThe difference between two singleand independent results, obtained by different operators work-ing in different laboratories on identical test material, would inthe long run, in the norma
37、l and correct operation of the testmethod, exceed the following value in only one case in twenty:0.3028 slopeNOTE 1The precision statement is based on the results from sevenlaboratories on six samples (see Table 1).10.2 BiasSince there is no accepted reference materialsuitable for bias determination
38、 of this test method, no statementon bias is being made.11. Keywords11.1 coolant; dispersion stability; emulsion; rolling oilANNEXES(Mandatory Information)A1. PREPARATION OF MIXING BEAKERA1.1 The mixing beaker3,4is a modification of a 5800 mLstainless beaker approximately 185 mm in diameter by220 mm
39、 high (see Fig. A1.1).A1.2 A piece of 6.35 mm outside diameter by 0.89 mm wallstainless tube is cut to 50 mm length, and the ends freed ofburrs or other irregularities. It is then brazed horizontally7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting
40、Research Report RR:D02-1108.FIG. 1 Tentative Dispersion Stability Test Report FormTABLE 1 Slope bLaboratory Test H I G K L JA 1 0.0 0.0031 0.9192 0.7188 0.4935 0.48222 0.0031 0.0 0.8757 0.6991 0.4986 0.4443B 1 0.0 0.0 0.5750 0.5264 0.7584 0.79382 0.0 0.0 0.5660 0.5410 0.6426 0.9548C 1 0.0274 0.0025
41、0.6133 0.8275 0.5725 0.60682 0.0046 0.0099 0.6759 0.8007 0.5949 0.4718D 1 0.0124 0.0513 0.8456 0.7530 0.4856 0.34272 0.0500 0.0 0.8077 0.7399 0.4047 0.5714E 1 0.0169 0.0128 0.3988 0.5793 0.6145 0.69702 0.0237 0.0169 0.3832 0.6152 0.5540 0.6970F 1 0.0158 0.0154 0.6050 0.5580 0.6640 0.97342 0.0338 0.0
42、097 0.6377 0.5653 0.9630 0.6779G 1 0.0428 0.0032 0.6393 0.5600 0.5111 0.46682 0.0301 0.0041 0.6531 0.5856 0.5458 0.5017D3342 90 (2017)3through the wall of the beaker, such that its center line is25 mm above the inside floor of the beaker, and it projects25 mm inside the wall (see Fig. A1.1).A1.3 A r
43、ectangle of sheet metal, 28.5 mm high by about76 mm wide, is brazed to the top of the beaker, on the sideopposite the sample tap, to permit attaching the control device,at a standard location (see Fig. A1.1).A1.4 A 76 mm piece of thin-walled rubber tube of suitableinside diameter to grip the 6.35 mm
44、 stainless tube, is slippedonto the outer end of that tube. It is fitted with a push-to-openspring-operated pinchcock, serving as a sampling valve.A2. PREPARATION OF SYNTHETIC HARD WATERA2.1 Prepare CaCl2solution of 50 000 ppm hardness. Froma freshly opened or carefully protected bottle of anhydrous
45、CaCl2, weigh out 55.5 g, and dissolve only in distilled water ina 1 L volumetric flask. (WarningMay cause skin irritation.)A2.2 Prepare MgSO4solution of 50 000 ppm hardness,using 123.2 g of MgSO47H2O per litre.A2.3 Prepare NaHCO3solution at 50 000 ppmconcentration, using 50 g of anhydrous NaHCO3per
46、litre.A2.4 For each litre of test water required, add to 994 mL ofdistilled water 3 mL of the CaCl2solution, 2 mL of the MgSO4solution, and 1 mL of the NaHCO3solution. Use Test MethodD1126 to verify hardness, if desired.A2.5 Adjust the pH of the hard water to 7.0 using dilutehydrochloric acid. (Warn
47、ingPoison. Corrosive. May be fatalif swallowed.) (See Test Methods D1293.)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 expressly advised that determination of the validity
48、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 withdrawn. Your comments
49、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 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, P
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