ASTM E1673-1996(2017) Standard Test Method for Percent Suspensibility《悬浮率百分比的标准试验方法》.pdf

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1、Designation: E1673 96 (Reapproved 2017)Standard Test Method forPercent Suspensibility1This standard is issued under the fixed designation E1673; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in

2、 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 is used to determine the percentsuspensibility of dry pesticide formulations.1.2 The values stated in SI units are to be regard

3、ed asstandard. No other units of measurement are included in thisstandard.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-priate safety and health practices and determine

4、 the applica-bility of regulatory limitations prior to use. For specificprecautionary statements see Section 7.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of I

5、nternational Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1126 Test Method for Hardness in WaterD1193 Specification for Reagent Water3. Summary of Test Method3.1 Aknown quantity of

6、 dry pesticide is slurried into 50 mLof test water in a 100-mL beaker. The slurry is quantitativelytransferred to a 250-mL mixing cylinder using additional testwater to rinse the beaker. The 250-mL mixing cylinder is thenfilled to volume with test water. The mixing cylinder isstoppered and inverted

7、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 is dried. The residueweight will determine the percent suspensibility.4. Significance and Use4.1 This test method is designed specifically for dryformulations,

8、 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 suspensibility.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

9、separation.4.4 This test method may not be applicable to formulationscontaining ingredients that decompose under the test condi-tions.4.5 This 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

10、volatile compo-nents may result in errors.5. Apparatus5.1 Balance, top loading, with an accuracy of 60.01 g orbetter.5.2 Beaker, 100 mL.5.3 Mixing Cylinder, stoppered, 250 mL, flat bottom, KI-MAX series 20039 or equivalent.5.4 Timer, adjustable, with an accuracy of 6 min.5.5 Magnetic Stirrer, 120 to

11、 1200 rpm, or equivalent.5.6 Stir Bar, magnetic 1 in. in length and38 in. in diameter(2.5 cm 1 cm).5.7 Weighing Dish, aluminum (57 18 mm) or petri dish, orequivalent.5.8 Vacuum Apparatus, see Fig. 1, equipped with a ventedstopper to prevent the formation of a vacuum.5.9 Filtering Flask, heavy wall,

12、500 mL, KIMAX Series27060 or equivalent.5.10 Gravity Oven.5.11 Centrifuge, any centrifuge capable of holding a 50 mLor larger tube and maintaining a minimum speed of 1500 rpm.1This test method is under the jurisdiction of ASTM Committee E35 onPesticides, Antimicrobials, and Alternative Control Agent

13、s and is the directresponsibility of Subcommittee E35.22 on Pesticide Formulations and DeliverySystems.Current edition approved April 1, 2017. Published April 2017. Originallyapproved in 1995. Last previous edition approved in 2012 as E1673 96 (2012).DOI: 10.1520/E1673-96R17.2For referenced ASTM sta

14、ndards, 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, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,

15、PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization

16、 Technical Barriers to Trade (TBT) Committee.15.12 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 thatall reagents shall conform to the specifications of th

17、e Commit-tee on Analytical Reagents of the American Chemical Societywhere such specifications are available.36.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean reagent water, Type IV, asdefined by Specification D1193.NOTE 1Type IV grade reagent water may be

18、prepared by distillation,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 app

19、roximately 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 carbonate to magn

20、esium carbonate.6.3.1 Soft WaterEquivalent to a total hardness of 34.2 ppmas calcium carbonate (CaCO3). Transfer 2.50 mL of synthetichard water stock by pipet to a 1000-mL volumetric flask anddilute to volume with water at 20C. Mix solution thoroughly.NOTE 2It is recommended that total hardness be c

21、hecked in accor-dance with Test Method MT-73, CIPAC 1, EDTA titration.4An alternatemethod is provided in Test Method D1126 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 carbonat

22、e (CaCO3). Transfer 25 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 har

23、d water stock by buret to a 1000-mL volumetricflask and dilute to volume with water at 20C. Mix this solutionthoroughly (see Note 2).6.3.4 Other Test WatersOther synthetic waters can beprepared by using the following calculation:Desired Water Hardness13.6805 (1)millilitres of synthetic hard water st

24、ock at 20Ctobediluted volumetrically to 1000 mL with water at 20C#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 preca

25、utions to prevent 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 respi-ratory devices approved by the National Institute of Occupa-tional Safety and Health (

26、NIOSH) for the product being tested.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 an

27、d stir with a magnetic 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.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC

28、. 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. (USPC), Rockville,MD.4“Analysis of Techn

29、ical and Formulated Pesticides,” CIPAC Handbook, Vol 1,compiled by Ashworth, R. de B., Henriet, J., Lovett, J. F., Collaborative Interna-tional Pesticide Analytical Council Ltd., Great Britain, 1970.FIG. 1 Vacuum ApparatusE1673 96 (2017)28.1.5 Fill the mixing cylinder to the 250 mL mark with testwat

30、er.8.1.6 Stopper and invert the mixing cylinder 15 completecycles, 2 s per cycle.8.1.7 Let the mixing cylinder stand for 30 min at 25C.Record ambient temperature. (See Note 3.)NOTE 3Other temperatures may be examined as defined by actualfield use applications.8.1.8 Remove the top 225 mL from the mix

31、ing cylinderusing 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 60.10 g.8.1.10 G

32、ently swirl the 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 60.10g and subtract the tare w

33、eight to determine 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 60.10 g.8.2.3 Transfer the sample into a 100-mL beaker containing50 mL of t

34、est water and stir 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 th

35、e mixing cylinder 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 sligh

36、tly below the liquidsurface 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 60.10 g.8.2.10 Gently swirl the remaining suspension to loosen thehard-packed material. Transfer quantitatively to the centrifuge

37、tube.8.2.11 Centrifuge 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

38、.2.11 in a 50C gravity oven to a constant weight.8.2.13 Weigh the centrifuge tube from 8.2.12 to an accuracyof 6 0.10 g 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 a

39、ccordance with product 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! 3100W1!(2)where:W1= sample weight, andW2= dried residue weight.11. Report11.1 Report percent susp

40、ensibility, ambient 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 o

41、f dupli-cate determinations, 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.

42、 Keywords13.1 dispersion; 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 methodsE1673 96 (2017)3ASTM International

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