1、Designation: E 1116 98 (Reapproved 2002)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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes a general procedure for thedetermination of emulsification spontanei
3、ty 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 follo
4、w all handling instructions for the specificformulation and conduct the test in accordance with goodlaboratory practice.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-pr
5、iate 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 in WaterD1193 Specification for Reagent Water3. Terminology3.1 Definitions:3.1.1 emulsification spontaneitythe rapid form
6、ation 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 spontaneity rating is assignedwhen the emulsion bloom (billowing) extends downward tonear the bottom of the water, with no visibl
7、e 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 the water and no free oilis present. Spontaneity descriptions between excellent and nil(no emulsion formed, only free oil) a
8、re 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), verygood, good, fair, and poor (nonhomogeneous) is assigned.3.1.3 DiscussionCream and oil separation may coexist.Normally, oil is
9、 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 liquid (because of partition and solubility properties) andcare must be taken to so note and record.3.1.4 Separation:3.1.4.1
10、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 nonemulsifiedliquid occurring at either the top or the bottom of the liquid.4. Summary of Test Method4.1 In this test method, emulsifi
11、able 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 terms of emulsion spontaneity,emulsion stability under static conditions, and re-emulsification of the coalesced phase.5. Sig
12、nificance and Use5.1 This test method provides a guide for evaluating emul-sification characteristics of pesticide emulsifiable concentrates.It defines the stability of emulsified particles in water.Althoughnot absolute, the test method is a measure of expected emulsionstability in agricultural appl
13、ication equipment.1This test method is under the jurisdiction of ASTM Committee E35 onPesticides and Alternative Control Agents and is the direct responsibility ofSubcommittee E35.22 on Pesticide Formulations and Delivery Systems.Current edition approved Oct. 10, 2002. Published March 2003. Original
14、lyapproved in 1986. Last previous edition approved in 1998 as E 1116 98.2For 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 AS
15、TM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Apparatus6.1 Analytical Balance, accurate to 0.01 g.6.2 Burets, 50 and 100-mL capacity.6.3 Graduated Cylinders, flat bottom, 100-mL capacity,glass stoppered, volume divisi
16、ons 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.36.4 Pipets, graduated serological, various delivery volumes.6.5 Pipet Filler, bulb-type or equivalent.6.6 Thermometer, graduated in 1 C increments and havinga minimum range from 0 to
17、 50 C.6.7 Volumetric Flasks, 1000-mL capacity calibrated at 20C.6.8 Constant Temperature (61 C) Device, of minimumvibration for housing 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
18、. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Societywhere such specifications are available.47.2 Pur
19、ity 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 water may be prepared by distillation,ion exchange, reverse osmosis, electrodialysis, or a combination thereof.7.3 Synthetic Ha
20、rd 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 reagents with approximately 750 mL ofwater and equilibrate to 20 C. Dilute the solution to 1000 mLtotal volume with water at 20 C
21、, 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 carbonate to magnesium carbonate.7.3.1 Soft Water, equivalent to a total hardness of 35 ppm ascalcium carbonate (CaCO3). Transf
22、er 2.6 mL of synthetic hardwater stock by pipet to a 1000-mL volumetric flask and diluteto volume with water at 20 C. Mix this solution thoroughly.NOTE 2It is recommended that total hardness as CaCO3be checked inaccordance with Test Method MT-73, CIPAC F, EDTA titration.5Analternate method is provid
23、ed 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 of 342 ppmas calcium carbonate (CaCO3). Transfer 26.0 mL of synthetichard water stock by buret to a 1000-mL volumetric flas
24、k anddilute to volume with water at 20 C. Mix this solutionthoroughly (Note 2).7.3.3 Extra-hard Water, equivalent to a total hardness of1000 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 20 C.
25、Mix thissolution thoroughly (Note 2).7.3.4 Other Test WatersOther synthetic waters can beprepared by using the following calculation:Desired Water Hardness 1 13.6805millilitres of synthetic hard water stock at 20 C to be dilutedvolumetrically to 1000 mL with water at 20 C.NOTE 3Soft water, hard wate
26、r, 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 100-mL graduated cylin-ders, 100 mL of 25C soft water, hard water, and extra-hardwater less the amount specified in 8.2.NO
27、TE 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 applications.8.2 Add a specified amount, in accordance with productlabel directions, of the test emulsifiable concentra
28、te at 25 C(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 rate shouldbe approximately 1 mL/s. Observe and record emulsificationspontaneity.8.3 Stopper the graduated cylinders (
29、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 25 C or at a constanttemperature (Note 4) and allow the cylinders to remainundisturbed. At 15 min, 30 min, 1 h, 2 h, and 24
30、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 outlined in 8.3. Return the cylinders to the 25C constant temperature device. At 30 min observe and recordthe emulsion quality
31、 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-tion, and subjectiveness of emulsion quality for the particularpesticide, no measurement of precision and bias can be mad
32、efor this test method.10. Keywords10.1 bloom; cream; emulsifiable concentrate; emulsifica-tion; pesticide; spontaneity3The glass cylinder available from Kontes Glass Co., Spruce St., Vineland, NJ08360, Model K-482500 has been found suitable. Equivalent cylinder from othersuppliers may be used.4“Reag
33、ent Chemicals, American Chemical Society Specifications,” AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see “Analar Standards for LaboratoryU.K. Chemicals,” BDH Ltd., Poole, Dorset, and the “United States Pharmacopoei
34、a.”5“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 (2002)2ASTM International takes no position respecting the validity of any patent rights ass
35、erted 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 revision at any time b
36、y 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 comments will rece
37、ive 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 Inte
38、rnational, 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 (2002)3
