ASTM E1673-1996(2006) Standard Test Method for Percent Suspensibility《百分比悬浮度标准试验方法》.pdf

1、Designation: E 1673 96 (Reapproved 2006)Standard Test Method forPercent Suspensibility1This standard is issued under the fixed designation E 1673; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number

2、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 is used to determine the percentsuspensibility of dry pesticide formulations.1.2 This standard does not purport to address a

3、ll of thesafety 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. For specificprecautionary statements see Section 7.2. Referen

4、ced Documents2.1 ASTM Standards:2D 1126 Test Method for Hardness in WaterD 1193 Specification for Reagent Water3. Summary of Test Method3.1 Aknown quantity of dry pesticide is slurried into 50 mLof test water in a 100-mL beaker. The slurry is quantitativelytransferred to a 250-mL mixing cylinder usi

5、ng additional testwater to rinse the beaker. The 250-mL mixing cylinder is thenfilled to volume with test water. The mixing cylinder isstoppered and inverted 15 complete cycles. The mixing cylin-der is allowed to stand for 30 min.After 30 min the top 225 mLis drawn off and the remaining suspension i

6、s dried. The residueweight will determine the percent suspensibility.4. Significance and Use4.1 This test method is designed specifically for dry formu-lations, but need not be restricted to these materials.4.2 Either option of this test method (see Section 8) may beused to determine the percent sus

7、pensibility.4.3 This test method may not be applicable to all dryformulations such as those containing either liquids or ingre-dients that rise to the top upon separation.4.4 This test method may not be applicable to formulationscontaining ingredients that decompose under the test condi-tions.4.5 Th

8、is test method may not give reproducible results ifflocculation occurs.4.6 This test method should be run in duplicate.4.7 Products containing water soluble or volatile compo-nents may result in errors.5. Apparatus5.1 Balance, top loading, with an accuracy of 60.01g orbetter.5.2 Beaker, 100 mL.5.3 M

9、ixing Cylinder, stoppered, 250 mL, flat bottom, KI-MAX series 200393or equivalent.5.4 Timer, adjustable, with an accuracy of 6 min.5.5 Magnetic Stirrer, 120 to 1200 rpm, or equivalent.5.6 Stir Bar, magnetic 1 in. in length and38 in. in diameter(2.5 cm 3 1 cm).5.7 Weighing Dish, aluminum (57 3 18 mm)

10、 or petri dish,or equivalent.5.8 Vacuum Apparatus, see Fig. 1, equipped with a ventedstopper to prevent the formation of a vacuum.5.9 Filtering Flask, heavy wall, 500 mL, KIMAX Series270603or equivalent.5.10 Gravity Oven.5.11 Centrifuge, any centrifuge capable of holding a 50 mLor larger tube and ma

11、intaining a minimum speed of 1500 rpm.5.12 Centrifuge Tube, plastic or glass, 50 mL or larger.6. Reagents (Test Water)6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended that1This test method is under the jurisdiction of ASTM Committee

12、E35 onPesticides and Alternative Control Agents and is the direct responsibility ofSubcommittee E35.22 on Pesticide Formulations and Delivery Systems.Current edition approved Nov. 15, 2006. Published December 2006. Originallyapproved in 1995. Last previous edition approved in 2001 as E 1673 96 (2001

13、).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.3Available from Fisher Scientific, 711 Forbes Avenue, Pitts

14、burgh, PA 15219.Also available from Curtin Matheson Scientific, Inc., P.O. Box 1546, Houston, TX77251-1546.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.all reagents shall conform to the specifications of the Commit-tee on Analytic

15、al Reagents of the American Chemical Societywhere such specifications are available.46.2 Purity of WaterUnless otherwise indicated, referenceto 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 distillatio

16、n,ion exchange, reverse osmosis, electrodialysis, or a combination thereof.6.3 Synthetic Hard Water StockTransfer 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 ofwat

17、er 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 carbonate to magnesium carbonate.6.3.1 S

18、oft WaterEquivalent to a total hardness of 34.2ppm as calcium carbonate (CaCO3). Transfer 2.50 mL ofsynthetic hard water stock by pipet to a 1000-mL volumetricflask and dilute to volume with water at 20C. Mix solutionthoroughly.NOTE 2It is recommended that total hardness be checked in accor-dance wi

19、th Test Method MT-73, CIPAC 1, EDTA titration.5An alternatemethod is provided in Test Method D 1126 where the value is representedas CaCO3. A value within 6 % of the nominal hardness value isacceptable.6.3.2 Hard WaterEquivalent to a total hardness of 342ppm as calcium carbonate (CaCO3). Transfer 25

20、 mL ofsynthetic hard water stock by buret to a 1000-mL volumetricflask and dilute to volume with water at 20C. Mix this solutionthoroughly (see Note 2).6.3.3 Extra-Hard WaterEquivalent to a total hardness of1000 ppm as calcium carbonate (CaCO3). Transfer 73.1 mL ofsynthetic hard water stock by buret

21、 to a 1000-mL volumetricflask and dilute to volume with water at 20C. Mix this solutionthoroughly (see Note 2).6.3.4 Other Test WatersOther synthetic waters can beprepared by using the following calculation:Desired Water Hardness 4 13.680 5millilitres of synthetic hard water stock at 20C to bedilute

22、d volumetrically to 1000 mL with water at 20C# (1)6.4 Other CarriersCarriers other than water may be usedwhen appropriate.7. Safety Precautions7.1 Before testing, read the precautionary statements on theproduct label or the Material Safety Data Sheet (MSDS), orboth. Take proper precautions to preven

23、t skin contact andinhalation of the fines or vapors, or both. Take care to preventcontamination of the surrounding area. Always wear theappropriate safety equipment and, where indicated, wear res-piratory devices approved by the National Institute of Occu-pational Safety and Health (NIOSH) for the p

24、roduct beingtested.8. Procedure8.1 Option A (Evaporation):8.1.1 Each sample should be run in duplicate.8.1.2 Weigh a 4-g sample into a weighing dish. Record thesample weight (W1) to an accuracy of 60.10g.8.1.3 Transfer the sample into a 100-mL beaker containing50 mL of test water and stir with a mag

25、netic stirrer at highspeed for two min.8.1.4 Quantitatively transfer the slurry from 8.1.3 into a 250mLmixing cylinder using up to 100 mLof additional test waterto rinse the beaker.8.1.5 Fill the mixing cylinder to the 250 mL mark with testwater.8.1.6 Stopper and invert the mixing cylinder 15 comple

26、tecycles, 2 s per cycle.8.1.7 Let the mixing cylinder stand for 30 min at 25C.Record ambient temperature. (See Note 3.)4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemica

27、l Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.5“Analysis of Technical and Formulated Pesticides,” CIPAC Handbook, Vol 1,compiled by Ashworth,

28、R. de B., Henriet, J., Lovett, J. F., Collaborative Interna-tional Pesticide Analytical Council Ltd., Great Britain, 1970.FIG. 1 Vacuum ApparatusE 1673 96 (2006)2NOTE 3Other temperatures may be examined as defined by actualfield use applications.8.1.8 Remove the top 225 mL from the mixing cylinderus

29、ing the vacuum apparatus in accordance with 5.8. Ensure thatthe tip of the suction tube remains slightly below the liquidsurface while removing the 225 mL. Take care not to disturbthe bottom 25-mL layer.8.1.9 Record the tare weight of the weighing dish to anaccuracy of 60.10g.8.1.10 Gently swirl the

30、 remaining suspension to loosen thehard-packed material. Transfer quantitatively to the weighingdish.8.1.11 Dry the weighing dish containing residue from 8.1.10in a 50C gravity oven to a constant weight.8.1.12 Weigh the dish from 8.1.11 to an accuracy of 60.10gand subtract the tare weight to determi

31、ne the dried residueweight (W2).8.2 Option B (Centrifuge/Evaporation):8.2.1 Each sample should be run in duplicate.8.2.2 Weigh a 4-g sample into a weighing dish. Record thesample weight (W1) to an accuracy of 60.10g.8.2.3 Transfer the sample into a 100-mL beaker containing50 mL of test water and sti

32、r with a magnetic stirrer at highspeed for 2 min.8.2.4 Quantitatively transfer the slurry from 8.2.3 into a 250mLmixing cylinder using up to 100 mLof additional test waterto rinse the beaker.8.2.5 Fill the mixing cylinder to the 250 mL mark with testwater.8.2.6 Stopper and invert the mixing cylinder

33、 15 completecycles, 2 s per cycle.8.2.7 Let the mixing cylinder stand for 30 min at 25C (seeNote 3). Record ambient temperature.8.2.8 Remove the top 225 mL from the mixing cylinderusing the vacuum apparatus in accordance with 5.8. Ensure thatthe tip of the suction tube remains slightly below the liq

34、uidsurface while removing the 225 mL. Take care not to disturbthe bottom 25-mL layer.8.2.9 Record the tare weight of the centrifuge tube to anaccuracy of 60.10g.8.2.10 Gently swirl the remaining suspension to loosen thehard-packed material. Transfer quantitatively to the centrifugetube.8.2.11 Centri

35、fuge the sample at a minimum speed of 1500rpm for 15 min or until the solution remaining above thepacked sediment appears free of any suspended particles.Gently decant the liquid, leaving as little as possible above thesediment.8.2.12 Dry the centrifuge tube with the sediment from8.2.11 in a 50C gra

36、vity oven to a constant weight.8.2.13 Weigh the centrifuge tube from 8.2.12 to an accuracyof 6 0.10g and subtract the tare weight to determine the driedresidue weight (W2).9. Disposal of Sample9.1 After testing, store all materials in a safe manner anddispose of used material in accordance with prod

37、uct labeldirections or MSDS, or both.10. Calculation10.1 Option A or B Calculations:10.1.1 Calculate % suspensibility of the insoluble materialas follows:% suspensibility 51093W12 W2! 3 100W1!(2)where:W1= sample weight, andW2= dried residue weight.11. Report11.1 Report percent suspensibility, ambien

38、t temperature,carrier, and option used.12. Precision and Bias12.1 RepeatabilityTwo results, each the mean of duplicatedeterminations, obtained by the same analyst should be con-sidered suspect if they differ by more than 3 % absolute.12.2 ReproducibilityTwo results, each the mean of dupli-cate deter

39、minations, obtained by analysts in different laborato-ries using the same option and sample weight should beconsidered suspect if they differ by more than 3 % absolute.12.3 BiasThis test method has no bias because the valueof suspensibility is defined only in terms of this test.13. Keywords13.1 disp

40、ersion; dry flowable; dry flowable test methods;percent suspensibility; suspension; water dispersible granules(WG) (WDG); water dispersible granules test methods; wet-table granules test methods; wettable powders (WP); wettablepowders test methodsASTM International takes no position respecting the v

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43、uarters. 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 shown below.This stan

44、dard 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).E 1673 96 (2006)3