1、Designation: E 1116 98 (Reapproved 2008)Standard Test Method forEmulsification Characteristics of Pesticide EmulsifiableConcentrates1This standard is issued under the fixed designation E 1116; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, 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 describes a general procedure for thedetermination of emulsification spontaneit
3、y and the emulsionstability characteristics of pesticide emulsifiable concentrateswhen diluted with water.1.2 Proper safety and hygiene precautions must be takenwhen working with pesticide formulations to prevent skin oreye contact, vapor inhalation, and environmental contamina-tion. Read and follow
4、 all handling instructions for the specificformulation and conduct the test in accordance with goodlaboratory practice.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thes
5、afety 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 use.2. Referenced Documents2.1 ASTM Standards:2D 1126 Test Method for Hardne
6、ss in WaterD 1193 Specification for Reagent Water3. Terminology3.1 Definitions:3.1.1 emulsification spontaneitythe rapid formation of anemulsion in the test water from agitation provided only by thegravity addition of the product. For products of density greaterthan the water used, an excellent spon
7、taneity rating is assignedwhen the emulsion bloom (billowing) extends downward tonear the bottom of the water, with no visible oil or creamdroplets reaching the bottom of the test cylinder. For productsof density less than the water used, a rating of excellent isgiven if bloom occurs near the top of
8、 the water and no free oilis present. Spontaneity descriptions between excellent and nil(no emulsion formed, only free oil) are assigned very-good,fair, and poor on a subjective basis.3.1.2 emulsion qualitya subjective evaluation of the emul-sion appearance. A rating of excellent (homogeneous), very
9、good, good, fair, and poor (nonhomogeneous) is assigned.3.1.3 DiscussionCream and oil separation may coexist.Normally, oil is located at either the extreme top or bottom ofthe liquid with cream between it and the rest of the emulsion.On rare occasions, separation occurs at both top and bottom ofthe
10、liquid (because of partition and solubility properties) andcare must be taken to so note and record.3.1.4 Separation:3.1.4.1 separation, creama discrete, opaque layer of con-centrated emulsion occurring at either the top or the bottom ofthe liquid.3.1.4.2 separation, oila discrete layer of nonemulsi
11、fiedliquid occurring at either the top or the bottom of the liquid.4. Summary of Test Method4.1 In this test method, emulsifiable pesticide concentratesare added to water of a given hardness and at a specifiedtemperature to form an oil-in-water emulsion. Performance ofthe formulation is measured in
12、terms of emulsion spontaneity,emulsion stability under static conditions, and re-emulsification of the coalesced phase.5. Significance and Use5.1 This test method provides a guide for evaluating emul-sification characteristics of pesticide emulsifiable concentrates.It defines the stability of emulsi
13、fied particles in water.Althoughnot absolute, the test method is a measure of expected emulsionstability in agricultural application equipment.6. Apparatus6.1 Analytical Balance, accurate to 0.01 g.6.2 Burets, 50 and 100-mL capacity.1This test method is under the jurisdiction of ASTM Committee E35 o
14、nPesticides and Alternative Control Agents and is the direct responsibility ofSubcommittee E35.22 on Pesticide Formulations and Delivery Systems.Current edition approvedOct. 1, 2008. Published November 2008. Originallyapproved in 1986. Last previous edition approved in 2002 as E 1116 98(2002).2For r
15、eferenced ASTM standards, visit the ASTM website, www.astm.org, orcontact 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,
16、West Conshohocken, PA 19428-2959, United States.6.3 Graduated Cylinders, flat bottom, 100-mL capacity,glass stoppered, volume divisions from 1 to 100 mL in 1-mLincrements, having an overall length of 300 6 15 mm and ahead space between 50 and 75 mm.6.4 Pipets, graduated serological, various delivery
17、 volumes.6.5 Pipet Filler, bulb-type or equivalent.6.6 Thermometer, graduated in 1C increments and having aminimum range from 0 to 50C.6.7 Volumetric Flasks, 1000-mL capacity calibrated at20C.6.8 Constant Temperature (61C) Device, of minimumvibration for housing graduated cylinders. This may be acon
18、trolled room, incubator, or a water bath of sufficient depthto allow immersion of graduated cylinders to above the100-mL mark.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifica
19、tions of the Commit-tee on Analytical Reagents of the American Chemical Societywhere such specifications are available.37.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water, Type IV, asdefined by Specification D 1193.NOTE 1Type IV grade reagent
20、water may be prepared by distillation,ion exchange, reverse osmosis, electrodialysis, or a combination thereof.7.3 Synthetic Hard Water Stock, transfer 12.14 g of anhy-drous calcium chloride (CaCl2) and 5.55 g of magnesiumchloride hexahydrate (MgCl26H2O) to a 1000-mL volumetricflask. Dissolve the re
21、agents with approximately 750 mL ofwater and equilibrate to 20C. Dilute the solution to 1000 mLtotal volume with water at 20C, stopper the flask and mix thesolution thoroughly. This mixture is equivalent to 13 680 ppmas calcium carbonate (CaCO3) and is based on a compositionalratio of 4:1 calcium ca
22、rbonate to magnesium carbonate.7.3.1 Soft Water, equivalent to a total hardness of 35 ppm ascalcium carbonate (CaCO3). Transfer 2.6 mL of synthetic hardwater stock by pipet to a 1000-mL volumetric flask and diluteto volume with water at 20C. Mix this solution thoroughly.NOTE 2It is recommended that
23、total hardness as CaCO3be checked inaccordance with Test Method MT-73, CIPAC F, EDTA titration.4Analternate method is provided in Test Method D 1126 where the value isrepresented as CaCO3. A value within 65 % of the nominal hardnessvalue is acceptable.7.3.2 Hard Water, equivalent to a total hardness
24、 of 342 ppmas calcium carbonate (CaCO3). Transfer 26.0 mL of synthetichard water stock by buret to a 1000-mL volumetric flask anddilute to volume with water at 20C. Mix this solutionthoroughly (Note 2).7.3.3 Extra-hard Water, equivalent to a total hardness of1000 ppm as calcium carbonate (CaCO3). Tr
25、ansfer 73.0 mL ofsynthetic hard water stock by buret to a 1000-mL volumetricflask and dilute to volume with water at 20C. Mix this solutionthoroughly (Note 2).7.3.4 Other Test WatersOther synthetic waters can beprepared by using the following calculation:Desired Water Hardness 1 13.6805millilitres o
26、f synthetic hard water stock at 20C to be dilutedvolumetrically to 1000 mL with water at 20C.NOTE 3Soft water, hard water, and extra-hard water may be preparedaccording to the World Health Organization (WHO) method WHO-M-13.R2. (approved Nov. 14, 1983).8. Procedure8.1 Transfer into three separate 10
27、0-mL graduated cylin-ders, 100 mL of 25C soft water, hard water, and extra-hardwater less the amount specified in 8.2.NOTE 4Other temperatures may be examined as defined by actualfield use applications.NOTE 5Other water hardnesses as described in 7.3.4 may be exam-ined as defined by actual field use
28、 applications.8.2 Add a specified amount, in accordance with productlabel directions, of the test emulsifiable concentrate at 25C(Note 4) to each cylinder. Deliver the emulsifiable concentrateusing a pipet from a height of 50 6 5 mm above the watersurface to the center of the water surface. Delivery
29、 rate shouldbe approximately 1 mL/s. Observe and record emulsificationspontaneity.8.3 Stopper the graduated cylinders (do not grease) theninvert and right each cylinder ten times at the rate of about onecomplete cycle every 2 s. Record the initial emulsion quality.8.4 Maintain each cylinder at 25C o
30、r at a constant tem-perature (Note 4) and allow the cylinders to remain undis-turbed. At 15 min, 30 min, 1 h, 2 h, and 24 h, observe andrecord the emulsion quality and the millilitres of cream or oilseparation, or both.8.5 After the 24-h observation, invert and right each cylin-der ten times as outl
31、ined in 8.3. Return the cylinders to the25C constant temperature device. At 30 min observe andrecord the emulsion quality and the millilitres of cream or oilseparation, or both.8.6 Discard the emulsions in a safe manner.9. Precision and Bias9.1 Due to the variability of cream separation, oil separa-
32、tion, and subjectiveness of emulsion quality for the particularpesticide, no measurement of precision and bias can be madefor this test method.10. Keywords10.1 bloom; cream; emulsifiable concentrate; emulsifica-tion; pesticide; spontaneity3Reagent Chemicals, American Chemical Society Specifications,
33、 AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc.
34、 (USPC), Rockville,MD.4“Hardness of Water,” Physico-Chemical Methods for Technical and Formula-tion Pesticides, Vol F, editors, Dobret W., Martin A., Collaborative InternationalPesticide Analytical Council Ltd., 1995.E 1116 98 (2008)2ASTM International takes no position respecting the validity of an
35、y 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 rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to rev
36、ision 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 revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your
37、 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 copyr
38、ighted 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).E 1116 98 (2008)3
