1、Designation: D 3707 89 (Reapproved 2005)e1An American National StandardStandard Test Method forStorage Stability of Water-in-Oil Emulsions by the Oven TestMethod1This standard is issued under the fixed designation D 3707; the number immediately following the designation indicates the year oforiginal
2、 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 moved into text editorially in May 2005.1. Scope1.1 T
3、his test method covers the stability of water-in-oilemulsions when held at a constant elevated temperature.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 conce
4、rns, 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 Documents2.1 ASTM Standards:2D 1744 Test Method for Water in Liquid P
5、etroleum Prod-ucts by Karl Fischer ReagentE 145 Specification for Gravity-Convection and Forced-Ventilation Ovens3. Summary of Test Method3.1 A 100-mL sample contained in a graduated 100-mLcylinder is placed in a thermostatically controlled oven at 85C(185F) for 48 or 96 h. The sample is then examin
6、ed for theamount of free oil and free water separated. In addition, watercontents of the sample at specified levels in the upper andlower layers of the sample are also obtained.4. Significance and Use4.1 This test method indicates the stability of the emulsionduring storage and normal usage.5. Appar
7、atus5.1 Convection Oven, meeting the requirements of Specifi-cation E 145.5.2 Graduated CylinderA stoppered 100-mL glass cylin-der graduated in 1-mL increments.3The stopper should have avent groove to prevent pressure buildup during the test.5.3 Pipet, 10-mL glass.5.4 Microsyringe, 0.05-mL glass wit
8、h 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 mixedthoroughly before removing the quantity required for the test.Vigorous hand shaking or mechanical mixing for 3 to 5 min isrecomm
9、ended 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 water-in-oil emulsions which are two-phase systemsas distinct from truly homogeneous systems. Vigorous me-chanical stirring for an
10、 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 representative sample.7. Test Method A48-h Test7.1 After careful preparation of the sample to obtain homo-geneity (described in
11、Section 6), transfer 100 mL to a gradu-ated 100-mL cylinder. Insert the vented stopper.7.2 Place the cylinder in a convection oven maintained at 856 1C (185 6 2F) for a period of 48 h. Take care to positionthe graduated cylinder in the oven generally in the center andraise at least 75 mm from the bo
12、ttom of the oven, to ensuretemperature uniformity.NOTE 1When carrying out a number of tests at the same time, arrangethe cylinders to avoid developing temperature variations in the oven due1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is th
13、e 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 3707 89 (1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cust
14、omer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3A “crows-foot” cylinder, British Standard BS 658, may be used.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
15、A 19428-2959, United States.to inadequate convection. The number of tests carried out at the same timeshould, for the same reason, also be restricted.7.3 Withdraw the cylinder from the oven and allow to standat room temperature, 21 6 3C (70 6 5F), for a period of 1h.7.4 Observe and record:7.4.1 The
16、amount of oil separated, percent volume and7.4.2 The amount of water separated, percent volume.7.5 By means of a 10-mL pipet, withdraw aliquots in thefollowing order:7.5.1 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 d
17、esignated as the upper layer sample.7.5.2 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.NOTE 2In the event that the amount of separated water equals orexceeds 10 % by volume then the
18、 determination of the water content ofthe lower layer is an optional procedure.7.6 Determine the water content, as percent weight, of theupper layer and lower layer samples, after shaking, by theprocedure given in the Annex. Use a 0.05-mL sample trans-ferred by means of a glass microsyringe.8. Test
19、Method B96-h Test8.1 This procedure is identical to that described underSection 7 except that the time period in the convection oven(7.2) is changed from 48 h to 96 h.9. Report9.1 Since the test can be performed on the basis of 48 h inthe oven (Test Method A) or 96 h (Test Method B), the reportis to
20、 indicate the procedure followed.9.2 Report the results as follows:9.2.1 Oil separation, percent volume,9.2.2 Water separation, percent volume,9.2.3 Upper layer water content, percent weight, and9.2.4 Lower layer water content, percent weight.10. Precision and Bias410.1 The precision (Note 3) of thi
21、s test method is dependenton the degree of stability of the emulsion, as follows:10.1.1 Type IStable Emulsions (Procedures A and B):10.1.1.1 The precision of the test method as determined bythe statistical examination of interlaboratory test results is asfollows.10.1.1.2 RepeatabilityThe difference
22、between successiveresults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould, in the long run, in the normal and correct operation ofthe test method, exceed the following values only in one casein twenty. (See Table 1.)10.1.1.3 Re
23、producibilityThe difference between twosingle and independent results obtained by different operatorsworking in different laboratories on identical test materialwould, in the long run, exceed the following values only in onecase in twenty. (See Table 1.)NOTE 3Precision limits are based on a round-ro
24、bin test programcarried out in Technical Division N in 1977 using invert emulsion sampleswith water contents between 35 and 50 % (weight). Eleven cooperatorstested five samples representing highly stable, borderline, and unstableemulsions.10.1.2 Type IIHighly Unstable EmulsionsThe precisionlimits fo
25、r the 96-h test are of the same order as for Type I. The48-h test would be less severe and less precise.10.1.3 Type IIIEmulsions of Borderline StabilityNoprecision limits can be set since the change in the samplestability with time or conditions, or both, of handling make itimpractical to determine
26、meaningful precision limits.10.2 BiasNo bias statement is possible because there is noabsolute value. The results are interpretable only with respectto this test.11. Keywords11.1 emulsions; oil separation; water separation4Supporting data have been filed at ASTM International Headquarters and maybe
27、obtained by requesting Research Report RR: D02-1158.TABLE 1 Repeatability and ReproducibilityFree Oil, % Free Water, %Difference in %Water ContentUpper Layer VersusLower LayerRepeatability 1 1 10Reproducibility 3 1 14D 3707 89 (2005)e12ANNEX(Mandatory Information)A1. MODIFIED TEST METHOD D 1744 (KAR
28、L FISCHER)A1.1 ScopeA1.1.1 This test method covers the determination of waterin the concentration from 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
29、 the product.A1.3 Modified ProcedureA1.3.1 To obtain weight of sample, weigh 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.
30、Harmful if inhaled. Skin irritant onrepeated contact. Eye irritant. Aspiration hazard.)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 noabsolute value. The resu
31、lts 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 validity of any such patent rig
32、hts, 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 are invited either for
33、 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
34、 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 3707 89 (2005)e13
