1、Designation: E1116 98 (Reapproved 2014)Standard Test Method forEmulsification Characteristics of Pesticide EmulsifiableConcentrates1This standard is issued under the fixed designation E1116; 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 describes a general procedure for thedetermination of emulsification spontaneity
3、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 a
4、ll 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 thesaf
5、ety 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:2D1126 Test Method for Hardness
6、in WaterD1193 Specification for Reagent Water3. Terminology3.1 Definitions:3.1.1 emulsification spontaneitythe rapid formation ofan emulsion in the test water from agitation provided only bythe gravity addition of the product. For products of densitygreater than the water used, an excellent spontane
7、ity rating isassigned when the emulsion bloom (billowing) extends down-ward to near the bottom of the water, with no visible oil orcream droplets reaching the bottom of the test cylinder. Forproducts of density less than the water used, a rating ofexcellent is given if bloom occurs near the top of t
8、he water andno free oil is present. Spontaneity descriptions between excel-lent and nil (no emulsion formed, only free oil) are assignedvery-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.3.1.2.1 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 ofth
10、e liquid (because of partition and solubility properties) andcare must be taken to so note and record.3.2 Separation:3.2.1 separation, creama discrete, opaque layer of con-centrated emulsion occurring at either the top or the bottom ofthe liquid.3.2.2 separation, oila discrete layer of nonemulsified
11、liquid 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 term
12、s 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 emulsified
13、 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 onPes
14、ticides, Antimicrobials, and Alternative Control Agentsand is the direct respon-sibility of Subcommittee E35.22 on Pesticide Formulations and Delivery Systems.Current edition approved Oct. 1, 2014. Published December 2014. Originallyapproved in 1986. Last previous edition approved in 2008 as E1116 9
15、8(2008).DOI: 10.1520/E1116-98R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International
16、, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.3 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, g
17、raduated serological, various delivery 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
18、 graduated cylinders. This may be acontrolled 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 r
19、eagents shall conform to the specifications 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 Specificati
20、on D1193.NOTE 1Type IV grade reagent 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 100
21、0-mL volumetricflask. Dissolve the reagents 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
22、 compositionalratio of 4:1 calcium carbonate 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 tho
23、roughly.NOTE 2It is recommended that total hardness as CaCO3be checked inaccordance with Test Method MT-73, CIPAC F, EDTA titration.4Analternate method is provided in Test Method D1126 where the value isrepresented as CaCO3. A value within 65 % of the nominal hardnessvalue is acceptable.7.3.2 Hard W
24、ater, equivalent to a total hardness 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
25、ppm as calcium carbonate (CaCO3). Transfer 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 W
26、ater Hardness113.6805millilitres of synthetic hard water stock at 20 C to be dilutedvolumetrically to 1000 mL with water at 20 C .#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. Proced
27、ure8.1 Transfer into three separate 100-mL graduatedcylinders, 100 mL of 25C soft water, hard water, andextra-hard water 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
28、-ined as defined by actual field use 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 c
29、enter of the water surface. Delivery 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
30、.8.4 Maintain each cylinder at 25C or 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 ri
31、ght each cylin-der ten times as outlined 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 variabil
32、ity of cream separation, oilseparation, and subjectiveness of emulsion quality for theparticular pesticide, no measurement of precision and bias canbe made for this test method.10. Keywords10.1 bloom; cream; emulsifiable concentrate; emulsifica-tion; pesticide; spontaneity3Reagent Chemicals, America
33、n Chemical Society Specifications, 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
34、.S. Pharmacopeial Convention, Inc. (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.E1116 98 (2014)2ASTM International takes no posit
35、ion 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 rights, and the riskof infringement of such rights, are entirely their own responsibilit
36、y.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 revision of this standard or for additional standardsand should be addressed to ASTM
37、 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 s
38、hown 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 98 (2014)3
