1、Designation: D 5145 03Standard Test Methods forNonvolatile and Pigment Content of Electrocoat Baths1This standard is issued under the fixed designation D 5145; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. 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 These test methods cover the characterization of elec-trocoat baths through the determination of nonvolatile contentof inorganic
3、 pigment content.1.2 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 the applica-bility of regulatory limitations prior to us
4、e.2. Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2D 2832 Guide for Determining Volatile and NonvolatileContent of Paint and Related Coatings3E 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial Chemicalsand Specialty Chem
5、icals43. Summary of Test Method3.1 Two specimens are accurately weighed into aluminumweighing dishes. The dishes are placed in an oven at 110C for1 h, reweighed to obtain the nonvolatile matter content and, ifrequired, placed in a muffle furnace at 500C for2handweighed a third time to obtain the ino
6、rganic pigment content.4. Significance and Use4.1 The nonvolatile content and pigment content are mea-sures of total solids and inorganic pigment solids, respectively,in electrocoat paints. In addition to production quality control,these properties are important in maintaining electrocoat bathsin th
7、e optimum range.4.2 Other test methods for determining nonvolatile contentof paint and paint related materials are described in GuideD 2832.5. Apparatus5.1 Analytical Balance with a sensitivity of 0.1 mg.5.2 Aluminum Weighing Dishes, 57 mm in diameter and 17mm deep. These commercial dishes may conta
8、in a lubricantused during their manufacture. This should be removed byheating the aluminum dishes on a hot plate at 300C untilvapors are no longer visible. Store the dishes in a desiccatoruntil needed.5.3 Syringes, 5-mL, disposable variety.5.4 Oven circulating, maintained at 110 6 2C.5.5 Muffle Furn
9、ace, maintained at 500 6 15C.6. Reagents6.1 Purity of WaterReferences to water shall be under-stood to mean water conforming to Type II of SpecificationD 1193.7. Sampling and Sample Preparation7.1 Obtain the sample while the electrocoat bath is underproper circulation so a uniform sample is obtained
10、. In the caseof a ultrafiltrate sample, the material should be thoroughlymixed or stirred prior to drawing the sample, thereby ensuringuniformity.7.2 After sampling, prior to removing the test specimen, it ismandatory the sample be shaken or stirred until it is homoge-neous and free of any settled m
11、aterial. This is particularlyimportant if there is a delay between sampling the bath andperforming this test procedure. The absence of settled materialshould be ascertained visually or by inserting a spatula andscraping the bottom of the container. Continue to shake or stirthe sample until specimens
12、 are taken for measurement. ThisPoint is Very Important.NONVOLATILE CONTENT8. Procedure8.1 Weigh two aluminum dishes separately, each to 0.1 mgand record as W1.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coating, Materials, and Applications and are the di
13、rect respon-sibility of Subcommittee D01.21 on Chemical Analysis of Paints and PaintMaterials.Current edition approved Jan. 10, 2003. Published March 2003. Originallyapproved in 1990. Last previous edition approved in 1997 as D 5145 - 90 (1997).2Annual Book of ASTM Standards, Vol 11.01.3Annual Book
14、of ASTM Standards, Vol 06.01.4Annual Book of ASTM Standards, Vol 15.05.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8.2 Using a syringe, withdraw 1.0 to 1.5 of the well mixedsample, then quickly weigh the syringe to 0.1 mg, record
15、ingthis weight as W2. Transfer the entire contents of the syringeinto the aluminum dish. Reweigh the empty syringe to 0.1 mgand record as W3. In the case of ultrafiltrate clear liquids or oflow solids paints, increase the specimen size to 5 mL andpreheat at 60C for 2 h. Duplicate this step with the
16、secondaluminum dish (8.1).8.3 Add a few millilitres of water to the specimen in thealuminum dishes prior to placing them in the oven. Thisfacilitates uniform spreading of the material. Place the dishesin the 110C oven for 1 h.8.4 Remove the dishes from the oven and allow to cool toroom temperature i
17、n a dessicator. Reweigh them to 0.1 mg andrecord the weights as W4.8.5 Retain the dishes for measurement of inorganic pigmentcontent as detailed in a following section of these test methods.9. Calculation9.1 Calculate the percent nonvolatile content as follows:% NV 5W42 W1W22 W33 100 (1)where:W1= we
18、ight of empty aluminum dish, g,W2= weight of syringe filled with sample, g,W3= weight of empty syringe, g, andW4= weight of dish and contents after1hat110C, g.10. Precision and Bias10.1 Precision is based on an interlaboratory study in whichthe operators in each of ten laboratories analyzed in dupli
19、cateon 2 days, four different electrocoat-bath samples with non-volatile contents ranging from 0.30 to 25.2 % The results wereanalyzed statistically in accordance with Practice E 180. Theinterlaboratory coefficient of variance was 1.6 % at 30 df andthe interlaboratory coefficient of variation was 2.
20、3 % at 27 df.Based on the these coefficients, the following criteria should beused for judging the acceptability of results at the 95 %confidence level:10.1.1 Repeatability: Two results, each the mean of dupli-cate determinations obtained by the same operator on differentdays, should be considered s
21、uspect if they differ by more than4.6 % relative.10.1.2 Reproducibility: Two results, each the mean of du-plicate determinations obtained by operators in different labo-ratories, should be considered suspect if they differ by morethan 6.7 % relative.10.2 Bias cannot be determined because there are n
22、o ac-cepted standards for nonvolatile content of electrocoat baths.INORGANIC PIGMENT CONTENT11. Procedure11.1 Place the weighing dishes used for the nonvolatilecontent determination in the muffle furnace at 500C for 2 h.11.2 After 2 h, remove the dishes from the muffle furnace,transfer them to a des
23、sicator and allow to cool to roomtemperature. After cooling, remove dishes and weigh to 0.1mg, recording these weights at W5.NOTE 1If an organic char is still present in the aluminum dish after 2h in the muffle furnace, continue heating in the furnace until no char ispresent.12. Calculation12.1 Calc
24、ulate the percent inorganic pigment as follows:% Inorganic Pigment EC Bath!5W52 W1W22 W33 100 (2)where:W1= weight of empty aluminum dish, g,W2= weight of syringe filled with sample, g,W3= weight of empty syringe, g, andW4= weight of aluminum dish and contents after heatingin muffle furnace, g.13. Pr
25、ecision and Bias13.1 Precision estimates are based on an interlaboratorystudy in which the operators in ten different laboratoriesanalyzed in duplicate on 2 days, four electrocoat bath materialscontaining inorganic pigment content ranging from 0.17 to4.52 weight %. The results were analyzed statisti
26、cally inaccordance with Practice E 180. The intralaboratory coefficientof variation was 2.2 % relative at 40 df and the interlaboratorycoefficient of variation was 10.8 % at 36 df. Based on thesecoefficients, the following criteria should be used for judgingthe acceptability of results at the 95 % c
27、onfidence level:13.1.1 Repeatability: Two results, each the mean of dupli-cate determinations, obtained by the same operator on differentdays, should be considered suspect if they differ by more than6.3 % relative.13.1.2 Reproducibility: Two results, each the mean of du-plicate determinations, obtai
28、ned by operators in different labo-ratories, should be considered suspect if they differ by morethan 31.1 % relative.13.2 Bias cannot be determined because there are no ac-cepted standards for inorganic pigment content of electrocoatbaths.14. Keywords14.1 electrocoat bath; muffle furnace; nonvolatil
29、e content;pigment content; ultrafiltratesD5145032ASTM 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 advised that determination of the validity of any such patent rights
30、, 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, either reapproved or withdrawn. Your comments are invited either for re
31、vision 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. If you feel that your comments have not received a fair hearing yo
32、u 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. 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).D5145033
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