1、Designation: D 6050 97 (Reapproved 2003)e1Standard Test Method forDetermination of Insoluble Solids in Organic LiquidHazardous Waste1This standard is issued under the fixed designation D 6050; 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.e1NOTEEquations 1 and 2 were corrected editorially in June 2003.1. Scope1.1 This test method covers the det
3、ermination of the ap-proximate amount of insoluble, suspended solid material inorganic liquid hazardous waste (OLHW).1.2 This test method is intended to be used in approximatingthe amount of insoluble, suspended solids in determining thematerial handling characteristics and fuel quality of OLHW. Iti
4、s not intended to replace more sophisticated procedures for thedetermination of total solids.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 prac
5、tices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D96 Test Methods for Water and Sediment in Crude Oil byCentrifuge Method (Field Procedure)23. Summary of Test Method3.1 A 10-mL aliquot of OLHW sample is decanted into a15-mL gradu
6、ated centrifuge tube and centrifuged for 3 min.The separated liquid phase of the OLHW is decanted into anappropriate waste vessel. The centrifuge tube with the sepa-rated solid material is brought back to its original 10-mLvolume with a user-selected blend of clean solvents andagitated to mix the so
7、lid and liquid phases. The tube iscentrifuged for 2 min, and the amount of remaining solidmaterial is read.4. Significance and Use4.1 Facilities utilizing bulk liquid hazardous waste fuels areconcerned about material handling characteristics and theoverall quality of the fuel. A high percentage of i
8、nsoluble,suspended solid material can create pumping, filtering, orgrinding difficulties in the off-loading of bulk shipments ofOLHW and can contribute to excessive wear on processingequipment. High solids can also decrease the quality andconsistency of commingled fuel by decreasing the effective-ne
9、ss of agitation in storage tanks.5. Apparatus5.1 CentrifugeCapable of spinning two or more centri-fuge tubes at a speed controlled to give a relative centrifugalforce of between 1200 to 1400. The speed to achieve this isgenerally between 3100 to 3600 rpm. The rotation speednecessary to achieve the r
10、elative centrifugal force can bedetermined from one of the following equations:rpm 5 1335rcfd(1)rpm 5 265rcfd(2)where:rpm = rotation speed, in revolutions per min,rcf = relative centrifugal force,d = diameter of swing, in mm (Eq 1) or in. (Eq 2),measured between the tips of opposite tubes whenthe tu
11、bes are in rotating position.NOTE 1Eq 1 and Eq 2 are described in Test Method D96.5.2 Centrifuge Tubes Centrifuge tubes shall be coneshaped, made of glass or a solvent resistant plastic or polymer,have a minimum capacity of 15 mL when filled to volume, andgraduated with minimum subdivisions of 0.5 m
12、L. Class Acentrifuge tubes are recommended. If any grade other thanClass A is used, refer to the section on Calibration andStandardization.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents con
13、form to the specifications of the Committee onAnalytical Reagents of the American Chemical Society where1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved March
14、10, 2003. Published June 2003. Originallyapproved in 1997. Last previous edition approved in 1997 as D 6050 97.2Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.such specifications are available.3Other grades may be used,pro
15、viding that it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Clean Solvent BlendThe user should formulate theclean solvent blend based on the “average” normal chemicalcomposition of the commingled OLHW. Th
16、e chemical compo-sition of OLHW is usually determined by gas chromatographicanalysis. The clean solvent blend will vary in complexitydepending on the specifications of the user.NOTE 2The clean solvent blend may be as simple as a singlecomponent (for example, toluene) or a complex mixture of aliphati
17、c andaromatic hydrocarbons, alcohols, esters, ketones, ethers, terpenoids, andhalogenated compounds. The user should formulate the clean solventblend based on compositional knowledge of the OLHW that the samplematerial is to be commingled with. If the commingled OLHW containswater, it may be appropr
18、iate to include in the clean solvent blend.7. Sample7.1 Because settling of insoluble solid material in liquidsamples is probable, the laboratory sample should be thor-oughly mixed by shaking prior to withdrawing a portion fortesting.8. Calibration and Standardization8.1 Centrifuge tubes other than
19、ClassAmust be periodicallychecked for accuracy. The frequency of this check will bedetermined by the user, but should be minimally done for eachnew box or lot number of tubes.9. Procedure9.1 Fill a centrifuge tube to the 10-mL graduation mark withthe OLHW sample.NOTE 3It will be necessary to use an
20、additional tube with an equalmass of water or other suitable liquid to balance the centrifuge.9.2 Place the tubes from 9.1 in the trunnion cups orcentrifuge tube slots on opposite sides of the centrifuge. Closethe centrifuge lid and engage safety lock, if so equipped.9.3 Set the centrifuge speed (r/
21、min) to provide a minimumrelative centrifugal force between 1200 to 1400 (see 5.1).9.4 Engage centrifuge, and allow to spin for 3 min.9.5 Remove the tube containing OLHW, and decant theseparated liquid phase to an appropriate waste vessel.9.6 Return the tube with solids to its original 10-mL volumew
22、ith the clean solvent blend. Cap or stopper the tube and shakevigorously in order to completely mix the centrifuged solidphase with the solvent phase. It may be necessary to use aVortex mixer for thorough mixing.9.7 Replace the OLHW tube in the centrifuge, and setcentrifuge as described in 9.2 and 9
23、.3.9.8 Engage centrifuge, and allow to spin for 2 min.9.9 Remove the OLHW tube, and decant the separatedliquid phase of each to an appropriate waste vessel.9.9.1 Visually estimate and record the amount of centri-fuged solids in the tubes to the nearest 0.25 mL.10. Quality Control10.1 Each laboratory
24、 using this test method will operate aformal quality control program. This program shall includeelements that address analyst proficiency through the evalua-tion of method blanks, duplicates, and reference materials ifavailable.11. Calculation11.1 The estimated amount of solid material is calculated
25、 asfollows:A/10 mL! 100 5 Insoluble solids, percent (3)where:A = volume of solids from centrifuge tube.12. Precision and Bias12.1 PrecisionThe precision of this test method is beingdetermined.12.2 BiasThe bias of this test method has not beendetermined because there are no recognized reference mater
26、i-als.13. Keywords13.1 centrifuge; hazardous waste; insoluble solids; organicliquid hazardous waste; suspended solidsASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly
27、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 by the responsible technical committee and must be reviewed every five years andif not revised, eit
28、her 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 receive careful consideration at a meeting of theresponsible technical committee, which you may attend
29、. 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Ind
30、ividual 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).3Reagent Chemicals, American Chemical Society Specifications, Am
31、ericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 6050 97 (2003)e12
