1、Designation: D 3709 89 (Reapproved 2005)e1An American National StandardStandard Test Method forStability of Water-in-Oil Emulsions Under Low to AmbientTemperature Cycling Conditions1This standard is issued under the fixed designation D 3709; the number immediately following the designation indicates
2、 the year oforiginal adoption or, 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.e1NOTEWarning notes were editorially moved into text in Ma
3、y 2005.1. Scope1.1 This test method covers the indication of the stability ofwater-in-oil emulsions when subjected to temperature cyclingchanges between ambient temperature and 18C (0F).1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is th
4、eresponsibility 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.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.2. R
5、eferenced Documents2.1 ASTM Standards:D 1744 Test Method for Water in Liquid Petroleum Prod-ucts by Karl Fischer Reagent23. Summary of Test Method3.1 A 100-mL sample contained in a graduated 100-mLcylinder is placed in a cooling box at 18C (0F) for 16 h andthen allowed to stand at room temperature f
6、or 8 h. This cyclingprocedure is repeated to give a total of nine cycles, except thatthe fifth cycle is one of 64 h at 18C (0F), 8 h at roomtemperature. At the completion of the cycling procedure thesample is examined for the amount of free oil and free waterseparated. In addition, water contents of
7、 the sample at specifiedlevels in the upper and lower layers of the sample are alsoobtained.4. Significance and Use4.1 This test method indicates the ability of the emulsion towithstand mild to moderately severe winter conditions of useand storage. Generally this significance would be limited tocond
8、itions where the emulsion reaches a minimum temperatureof 18C (0F).5. Apparatus5.1 Cold BoxAthermostatically controlled freezer or coldbox capable of being maintained at 18 6 1.5C (0 6 3F).5.2 Graduated CylinderA stoppered 100-mL glass cylin-der graduated in 1.0-mL increments. The stopper should hav
9、ea vent groove to prevent vacuum or pressure build-up duringthe test.5.3 Pipet, 10-mL glass.5.4 Microsyringe, 0.05-mLglass with a fixed needle, No. 19gage, point style No. 3.5.5 Glass Vials, approximately 30-mL size.6. Preparation of Sample6.1 To ensure uniformity of the sample, it should be mixedth
10、oroughly before removing the quantity required for the test.Vigorous hand shaking or mechanical mixing for 3 to 5 min isrecommended for litre-size containers or less.6.2 Special difficulties arise in mixing and withdrawingrepresentative samples from large containers. This is due to thenature of wate
11、r-in-oil emulsions that are two-phase systems asdistinct from truly homogeneous systems. Vigorous mechani-cal stirring for an extended period is the best means ofachieving homogeneity. However, for unstable emulsions thathave been in storage for some time there is no satisfactory wayto obtain a repr
12、esentative sample.7. Procedure7.1 After careful preparation of the sample to ensure homo-geneity (described in Section 6), transfer 100 mL to a gradu-ated 100-mL cylinder. Insert the vented stopper.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants
13、and is the direct responsibility of SubcommitteeD02.N0 on Hydraulic Fluids.Current edition approved May 1, 2005. Published May 2005. Originallyapproved in 1978. Last previous edition approved in 1999 as D 3709 89 (1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
14、ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.2 Place the cylinder in
15、the cold box at 18 6 1.5C (0 63F) for a period of 16 h. Withdraw the cylinder from the coldbox and allow to stand at room temperature, 21 6 3C (70 65F), for a period of 8 h.7.3 Repeat the cycling procedure as in 7.2 for three morecycles.7.4 Replace the cylinder in the cold box for a period of 64h. W
16、ithdraw and allow to stand at room temperature for 8 h.7.5 Repeat the cycling procedure as in 7.2 for four morecycles, except that during the final cycle, the period at roomtemperature is limited to 3 h instead of 8 h before makingobservations.7.6 Observe and record the following:7.6.1 The amount of
17、 oil separated, percent volume, and7.6.2 The amount of water separated, percent volume.7.7 By means of a 10-mL pipet, withdraw aliquots in thefollowing order.7.7.1 With the pipet tip located exactly at the 80-mL mark,slowly withdraw a 10-mL sample and transfer to a small glassvial. This is designate
18、d as the upper layer sample.7.7.2 With the pipet tip located exactly at the 15-mL mark,slowly withdraw a 10-mL sample and transfer to a small glassvial. This is designated as the lower layer sample.7.8 Determine the water content, as percent weight, of theupper layer and lower layer samples, after s
19、haking, by theprocedure given in the Annex. Use a 0.05-mL sample trans-ferred from the vials by means of a glass microsyringe.8. Report8.1 Report the results as follows:8.1.1 Oil separation, percent volume,8.1.2 Water separation, percent volume,8.1.3 Upper layer water content, percent weight, and8.1
20、.4 Lower layer water content, percent weight.9. Precision and Bias39.1 The precision (see Note 1) of this test method isdependent on the degree of instability brought about by thetemperature cycling process.9.1.1 Type IStable Emulsions (Procedures A and B):9.1.1.1 PrecisionThe precision of the metho
21、d as deter-mined by the statistical examination of interlaboratory testresults is as follows.9.1.1.2 RepeatabilityThe difference between successiveresults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould, in the long run, in the
22、 normal and correct operation ofthe test method, exceed the following values only in one casein twenty. (See Table 1.)9.1.1.3 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would, i
23、nthe long run, exceed the following values only in one case intwenty. (See Table 1.)NOTE 1Precision limits are based on a round-robin test programcarried out in Technical Division N in 1977 using invert emulsion sampleswith water contents between 35 and 50 % (weight). Eleven cooperatorstested five s
24、amples representing highly stable, borderline, and unstableemulsions.9.1.2 Type IIUnstable Emulsions Results can varywidely on samples which show any degree of instabilitybrought about by temperature cycling and no precision limitscan be set.9.1.3 BiasNo bias statement is possible because there isno
25、 absoute value. The results are interpretable only withrespect to this test.10. Keywords10.1 emulsions; oil separation; water separationANNEX(Mandatory Information)A1. MODIFIED TEST METHOD D 1744 (KARL FISCHER)A1.1 ScopeA1.1.1 This test method covers the determination of waterin the concentration fr
26、om 50 to 1000 ppm in liquid petroleumproducts.A1.2 Significance and UseA1.2.1 Knowledge of the water content of petroleum prod-ucts can be useful to predict quality and performance charac-teristics of the product.3Supporting data have been filed at ASTM International Headquarters and maybe obtained
27、by requesting Research Report RR: D02-1158.TABLE 1 Repeatability and Reproducibility For Type 1 OnlyFree Oil, % Free Water, %Difference in %Water ContentUpper Layer VersusLower LayerRepeatability 1 1 3Reproducibility 2 2 3D 3709 89 (2005)e12A1.3 Modified ProcedureA1.3.1 To obtain weight of sample, w
28、eigh the syringe to 0.1mg before and after introducing the sample to the titrationvessel.A1.3.2 Use a 1 part xylene to 2 parts methanol mix as thesolvent instead of a 3 parts chloroform to 1 part methanol mix.(WarningFlammable. Harmful if inhaled. Skin irritant onrepeated contact. Eye irritant. Aspi
29、ration hazard.)A1.3.3 A water equivalent of 2.0 to 2.5 mg of water/mL forthe Karl Fischer reagent is recommended.A1.4 Precision and BiasA1.4.1 The precision of Test Method D 1744 with thissolvent system is now under study by Subcommittee D.02.03.A1.4.2 No bias statement is possible because there is
30、noabsolute value. The results are interpretable only with respectto this test.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 valid
31、ity 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 comme
32、nts 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 n
33、ot 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).D 3709 89 (2005)e13
