DETERMINATION OF VOLUME SOLIDS OF PAINTS AND
DETERMINATION OF VOLUME SOLIDS OFPAINTS AND COATINGSBY ACCURATE DRY FILM THICKNESS MEASUREMENTSMARCH, 1981Prepared by:Georgia Institute of TechnologyEngineering Experiment Stationin cooperation withAvondale Shipyards, Inc.
Form ApprovedOMB No. 0704-0188Report Documentation PagePublic reporting burden for the collection of information is estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources, gathering andmaintaining the data needed, and completing and reviewing the collection of information. Send comments regarding this burden estimate or any other aspect of this collection of information,including suggestions for reducing this burden, to Washington Headquarters Services, Directorate for Information Operations and Reports, 1215 Jefferson Davis Highway, Suite 1204, ArlingtonVA 22202-4302. Respondents should be aware that notwithstanding any other provision of law, no person shall be subject to a penalty for failing to comply with a collection of information if itdoes not display a currently valid OMB control number.1. REPORT DATE2. REPORT TYPEMAR 1981N/A3. DATES COVERED-4. TITLE AND SUBTITLE5a. CONTRACT NUMBERDetermination of Volume Solids of Paints and Coatings by Accurate DryFilm Thickness Measurements5b. GRANT NUMBER5c. PROGRAM ELEMENT NUMBER6. AUTHOR(S)5d. PROJECT NUMBER5e. TASK NUMBER5f. WORK UNIT NUMBER7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES)Naval Surface Warfare Center CD Code 2230 - Design Integration ToolsBuilding 192 Room 128 9500 MacArthur Bldg Bethesda, MD 20817-57009. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES)8. PERFORMING ORGANIZATIONREPORT NUMBER10. SPONSOR/MONITOR’S ACRONYM(S)11. SPONSOR/MONITOR’S REPORTNUMBER(S)12. DISTRIBUTION/AVAILABILITY STATEMENTApproved for public release, distribution unlimited13. SUPPLEMENTARY NOTES14. ABSTRACT15. SUBJECT TERMS16. SECURITY CLASSIFICATION OF:a. REPORTb. ABSTRACTc. THIS PAGEunclassifiedunclassifiedunclassified17. LIMITATION OFABSTRACT18. NUMBEROF PAGESSAR4119a. NAME OFRESPONSIBLE PERSONStandard Form 298 (Rev. 8-98)Prescribed by ANSI Std Z39-18
TABLE OF CONTENTSPageLIST OF FIGURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iiLIST OF TABLES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iiiFOREWORD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ivEXECUTIVE SUMMARY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . viSection1.CONCLUSIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12.PROJECT PLAN OF ACTION AND RESULTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32.1 Objective . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32.2 General Approach . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32.2.1 New, Proposed Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42.3 Plan of Action . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112.3.1 Scope of Work. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112.3.2 Statement of Work . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132.4 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 162.4.1 Discussion of the Volume Solids results obtained byusing the ASTM D 2697-73 Method . . . . . . . . . . . . . . . . . . . .162.4.2 Discussion of the Volume Solids results obtained byusing the Film Thickness Measurement Method . . . . . . . . . . 192.4.3 Discussion of the Volume Solids Values based on theresults obtained by altering the during temperaturesin ASTM D 2697-73 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192.4.4 Comparison of the ASTM D 2697-73 Method and the filmthickness method for obtaining volume solids . . . . . . . . 193.Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
LIST OF FIGURESPageFigure 1.Schematic representation of the research plan . . . . . . . . . . . . . .12Figure 2.Example volume solids determination by film thicknessmethod . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17Figure 3.Diagram of spinning apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 ii
LIST OF TABLESPageTable 1.Precision and accuracy of some film thickness measurements . .9Table 2.Precision of some film thickness measurements . . . . . . . . . . . . . . . .10Table 3.Volume solids as determined by the ASTM D 2697-73 StandardMethod . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23Table 4.Volume solids as determined by the film thickness measurementMethod . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25Table 5.Comparison of volume solids results by altering the ASTM D2697-73 method curing temperatures . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27Table 6.Student’s t-test of Statistical Significance between ASTM D2697-73 and film thickness method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
FOREWORDAvondale Shipyards, Inc. has been contracted by the U.S. Departmentof Commerce, Contract No. 5-38071, to manage its research and developmentefforts in the area of surface preparation and coating.Pursuant with this responsibility, the following research and development was sub-contracted to the Engineering Experiment Station, GeoraiaInstitute of Technology.“Development of a Standard Procedure for Determining Volume Solids of Coatings.”This research project was undertaken with the primary objective asthe development of a standard analytical procedure to determine the volumesolids of liquid coatings.The volume solids obtained was to accuratelyrepresent the volume of dried coating film (coverage) obtained from a gallonof liquid material.Successful completion of the work would, at least, provide a detailedprocedure for measuring the volume solids of coatings used in the marineindustry.Once these procedures are adopted by the marine industry, coatingsuppliers can be required to report the volume solids on that basis andnot values calculated from a formula sheet.This would help in estimatingthe quantity of paint required for various jobs, minimizing the probabilityof purchasing too little or too much paint with obvious dollar savings.With better volume solids data, the estimate of painting time can also bemade more accurately using, for example, the effective solids output parameter promoted by Ginsberg.lMr. Leslie E. Henton, of the Engineering Experiment Station, servedas Princ pal Investigator. Mr. Wayne Case, of the same institute, performediv
all testing operations.On behalf of Avondale Shipyards, Inc., Mr. JohnPeart was the R & D Project Manager responsible for technical direction,editing, and publication of this report.Special thanks are given to Mr. David Hurst, of the EngineeringExperiment Station, Georgia Institute of Technology, for the film thicknessmeasurement concept and to Mr. W. R. Tooke, Jr. of Micro-Metrics Companyfor supplying data from an ASTM round robin on dry film measurements. Also,we wish to acknowledge the contributions of the following corporations:Avondale shipyards, Inc., New Orleans, LouisianaCarboline Marine Corporation, St. Louis, MissouriFarboil Company, Baltimore, MarylandGeneral Polymers Corporation, Cincinnati, OhioImperial Coatings Corporation, New Orleans, LouisianaInternational Paint Company, Inc., Union, New JerseyJotun-Baltimore Copper Paint Company, Baltimore, MarylandMatcote Company, Inc., Houston, TexasNAPCO Corporation, Houston, TexasPorter Coatings, Louisville, KentuckySigma Coatings, Harvey, LouisianaV
EXECUTIVE SUMMARYA new method to determine the volume solids of paints and coatingsbased on the measurement of dried film thickness over a known area hasbeen studied in this work.It was compared to the American Society forTesting and Materials Method D 2697-73 Volume Nonvolatile Matter in Clearand Pigmented Coatings.This method determines the volume of the dry filmby application of the Archimedes buoyancy effect. In addition, the projectwas structured to extend the ASTM method to coatings systems used in themarine industry.The volume solids of several typical marine coating systems were determined using the proposed film thickness method as well as the current ASTMmethod.The type of coatings examined were ketimine cured epoxies, amineand amine adduct cured epoxies, polyamide cured epoxies, vinlys, chlorinatedrubbers, alkyds, inorganic zinc-rich coatings, urethanes, and waterbornecoatings.The film drying or curing conditions used were appropriate tothe chemistry involved in the film forming process.The results indicate that the precision of the ASTM method is betterthan the precision of the film thickness method. This is primarily dueto poor film thickness uniformity.It was also shown that there is nobenefit in time savings and sample handling in making volume solids determinations by the film thickness technique, when the manufacturer’s recommendedconditioning schedule is used to cure the paint film. The ASTM Method,then is the preferred one.From the results of the work on this project, it is concluded thatthe user and the paint supplier must agree upon the curing or conditioningschedule, as the curing conditions can affect the volume solids valuesobtained.
Any further work done in pursuing the film thickness technique shouldbe in the direction of obtaining a method that will give samples withuniform film thickness.vii—.
SECTION 1Conclusions
CONCLUSIONS1.The precision in the film thickness method is much less than the precision of the ASTM method.This is due to the lack of film thicknessuniformity.2.There is no benefit in time savings and sample handling in making avolume solids determination by the film thickness method in comparisonwith the ASTM method.3.The curing conditions can affect the volume solids values obtainedso it is imperative that the manufacturer and user agree upon the conditioning schedule.4.This is already recognized in the ASTM method.Although there were cases where the volume solids values obtained bythe two methods agreed in terms of the student’s t-test, the largevariances in the film thickness method may negate the validity of thoseagreements.7
SECTION 2Project Plan ofAction and Results
2. PROJECT PLAN OF ACTICN AND RESULTS2.1 ObjectiveThe objective was development of a standard analytical procedure fordetermining the volume solids of liquid coatings. The volume solids obtainedwas to accurately represent the volume of dried coating film (coverage) obtained from a gallon of liquid material.2.2 General ApproachThe present ASTM method for the determination of the volume solidsof clear and pigmented coatings, ASTM D 2697-73,2 is based on the indirectmeasurement of the volume of a dried paint film using the Archimedesbuoyancy effect.The weight of the paint film, supported on a metalsubstrate, is determined in air and in some liquid of known specificgravity.The weight (mass) difference divided by the specific gravityof the liquid gives the volume of the paint film. This data in combination with the weight solids and the specific gravity of the wet paint isthen used to calculate the volume solids.In principal, this method ishighly accurate since it is based on well established gravimetric techniques.The method, however, is not used widely in the coatings industry. Volumesolids typically are calculated from formulations or batch sheets usingthe density of the individual components and assuming that the volumes areadditive.This assumption is, in general, incorrect. Hence, experimentalvolume solids and calculated volume solids will be different; the maqnitudeof this difference will be dependent on the magnitude of the error inassuming that the volumes are additive.There are sources for error or differing interpretations to theapplication of ASTM D 2697-73 to the wide range. of paints and coatingsfound In industry.One must determine if, for example, voids or pores
are a proper part of the final film structure for, ifSO,a liquid mustbe used that will not penetrate into these voids. The displacement liquidsused must also not be absorbed into the paint film, at least in the timeit takes to make the weight measurements.Reasonable, intelligent modifi-cations to the method must also be made based on the chemistry involvedin the film forming process for each coating tested. Here, a particularlysensitive point is the conditioning procedures for obtaining a final driedfilm and the determination of the weight non-volatiles of the coating.The current method recommends drying for three hours at 105 C although thisis qualified by a note which identifies the best drying conditions as thoserecommended by the manufacturer of the coating and similar to the in-usecuring conditions.Unintentional abuses of the drying procedure have occurred.For example, a coating based on unsaturated polyester cured or crosslinkedby in-situ, room temperature polymerization with styrene was subjectedto the 105 C heating.3This, of course, volatilized the styrene, a normalcomponent of the dried coating, which lead to completely erroneous results.Similar problems can be expected in systems that use low molecular weightmatrials that are crosslinked into the final film by reaction with absorbedwater vapor such as urethane systems or ketimine-epoxy systems. It seemsobvious, at this point that for the wide range of coatings used in themarine industry appropriate methods of film drying or curing for 2.2.1.News, Proposed MethodsA method to determine the volume solids of paints and coatings basedon the measurement of dried film thickness has been studied in this work.The method does not require the selection of a displacement liquid so thaterrors due to the penetration or non-penetration of the liquid into poresand/or voids and the swelling/absorption properties of the coating-liquid4
system are avoided.The new method entails the measurement of the weight of the wet,freshly applied coating, the specific gravity of the wet coating, and itsdry film thickness over a known area.Drying or curing conditions areselected appropriate to the coating system.The volume solids, , of a paint or coating in this alternate methodis given by(1)the wet paint, and W is the weight of the wet coating applied to area A.That is, the initial volume of paint applied is(2)and the final volume isVf AT(3)In any experimental determination of a quantity, there are errors inthe measurements which introduce uncertainties into the final, calculatedvalue.The error analysis of the film thickness measurement technique per-formed here is based on a standard propagation of errors approach.4 Itrepresents the largest error in the volume solids one can reasonably expect.The limit of error in the volume solids,is given by
(4)whererepresent the limit of error for eachof the measured quantities.On a relative basis, the limit of erroris(5)i.e., the relative limit of error of the volume solids is equal to the sumof the relative limit of error for each experimentally determined quantity.The limit of error in the density,can be taken as the limitspecified in ASTM D 1475 Density of Paint Varnish, Lacquer and RelatedProducts since this method is used.b The value of the limit is 0.915 lb/gal.(0.002 kg/L) which represents 30 (u is the variance) limits. Using thedensity of water as 8.331b/qal as a reference point, the relative errorlimit is O.2 per cent.Since most piqmented paints will have a densitygreater than that of water, the relative error value of 0.2 per cent isprobably an upper limit.The relative error in the weight of the wet sample is expected tobe extremely small since the weight, determined to a tenth of a milligram(0.1 mg.), is on the order of 100 mg.order of 0.1 per cent.This gives a relative error on theThis error, of course, may be larger depending on thevolatility of the solvent blend in any particular paint. If rapid weight
The errors associated with the area of the dish holding the wet anddry paint can be made small by using evaporating dishes which are constructedof aluminum and have smooth, flat bottom. and nearly vertical sides. 7 Ifthe nominal 50 mm diameter is accurate to O.1 mm, the relative error becomesO. 2mm—----50 mm 0.004(6)Again, one can reasonably expect a maximum error on the order of a fewtenths of a per cent.The accurate measurement of film thickness is the critical part ofthe proposed approach to volume solids measurements. For the factorsbriefly explored above, the cumulative, relative error is 1 per cent asa maximum.For a first look at the film thickness precision, one canuse data supplied on rough ASTM methods of film thickness measurement.If a non-magnetic sample cup is used, an instrument based on eddy currentsinduced in the substrate metal can be used.From an ASTM D 1400-67 roundrobin testing with eddy current instruments, the standard deviation betweenresults from different laboratories was 0.11 mil.8If 1.96G is takenas the limit for the error, (95 per’cent confidence limits), the limitof relative error is(7)using 3 roils as a typical film thickness.It should be noted that the “in lab” standard deviation was 0.0557
mil; this reduces the error limit to “4 per cent in equation (7).Keane and Shoemaker have reported on film thickness measurementsfor coatings on structural steel using various magnetic gages.g Theyconclude that the instruments are inherently accurate to within 15 percent of the true thickness and that the accuracy is improved by severalthickness determinations and averaging.This can also be seen in datareported below.Table 1 contains the analysis of film thickness measurements usingtwo different, commercial magnetic gages. This data was supplied byW. R. Tooke, Jr.of the Micro-Metrics CompanyIn Table 1, the averagefilm thickness, the per cent error defined asand the per cent relative error limit defined as(9are reported.The limit of error is taken as 1.96;for a normal dis-tribution this represents the 95 per cent confidence limit.8
Table 1.Precision and— Accuracy— . — — . — of Some Film Thickness MeasurementsInstrumentNominal FilmThickness (mill)Zorelco a747-FZorelco 747-NFVerimeter bAverage FilmThickness .003.40.3138.84.735.3().712137.708.20.46.54.9
Table 2.Precision of Some Film Thickness MeasurementsPanel Area21Instrument3Minitector a(6.3 0.l/2.316.3 0.7/4.31.2 0.2/17Verimeter b6.1 0.1/1.615.7 0.5/3.21.3 0.2/15a Zormco Electronics Corporation, 8520 Garfield Blvd., Cleveland, Ohio44125; telephone: 216-441-610030324 ;b Micro-Metrics Company, P. O. Box 13804, Atlanta, Georgiatelephone: 404-325-3243.The data supplied by W. R. Tooke, Jr. of Micro-Metrics Company, waspart of an ASTM round robin on dry film measurement. The average valuereported is for six film thickness values measured in sets of threaontwo consecutive days.The precision is much better than that reported inTable 1, reflecting a better sample size and better calibrating procedures.The higher relative error for thin film, i.e., those1 mil, reflect thegreater difficulty in determining the thickness of thin films. The absolute limit of error is still small: 0.2 mil. Since most marine coatingsare used at thicknesses
The present ASTM method for the determination of the volume solids of clear and pigmented coatings, ASTM D 2697-73, 2 is based on the indirect measurement of the volume of a Author: Leslie E Henton, Wayne Case
1. Total solids (Standard Methods 2540B) 2. Total solids after screening with a 106 µm sieve 3. Total suspended solids (solids retained on a 0.45 µm filter) (Standard Methods 2540D) 4. Total Dissolved Solids (solids passing through a 0.45 µm filter) (Standard Methods 2540C) 5. Turbidity using a HACH 2100N Turbidimeter 6.
SDI sludge density index . SRT solids retention time . SS settleable solids . SSV. 30. settled sludge volume 30 minute . SVI sludge volume index . TOC total organic carbon . TS total solids . TSS total suspended solids . VS volatile solids . WAS waste activated sludge . Conversion Factors: 1 acre 43,560 square feet . 1 acre foot 326,000 .
ENVIRONMENTAL ENGINEERING LABORATORY – SYLLABUS Exp. No. Name of the Experiment 1. Determination of pH and Turbidity 2. Determination of Conductivity and Total Dissolved Solids (Organic and Inorganic) 3. Determination of Alkalinity/Acidity 4. Determination of Chlorine 5. Determination of Iron 6. Determination of Dissolved Oxygen 7.
Solids 1.1 Classification of solids 8 1.2 Crystalline solids – structure and properties 8 1.3 Amorphous solids 25 1.4 Dissolution of solid drugs 26 1.5 Importance of particle size in the formulation and manufacture of solid dosage forms 28 1.6 Biopharmaceutical importance of particle size 29 1.7 Wetting of powders 31 1.8 Sublimation 34
concentration or total suspended solids. Analytical methods for determination of suspended-sediment concentration and total suspended solids are different. For water samples that contain large particles (sand size or greater), the reported value of total suspended solids may be slightly less than the value reported for total suspended sediment.
Find the volume of each cone. Round the answer to nearest tenth. ( use 3.14 ) M 10) A conical ask has a diameter of 20 feet and a height of 18 feet. Find the volume of air it can occupy. Volume 1) Volume 2) Volume 3) Volume 4) Volume 5) Volume 6) Volume 7) Volume 8) Volume 9) Volume 44 in 51 in 24 ft 43 ft 40 ft 37 ft 27 .
Notes on Activated Sludge Process Control Page ii Total solids are defined as all the matter that remains as residue upon evaporation at 103 to 105 oC. Total solids can be classified as either suspended solids or filterable solids by passing a known volume of liquid th
Grade 2 Writing and Language Student At-Home Activity Packet 3 Flip to see the Grade 2 Writing and Language activities included in this packet! This At-Home Activity Packet is organized as a series of journal entries. Each entry has two parts. In part 1, the student writes in response to a prompt. In part 2, the student completes a Language Handbook lesson and practices the skill in the .
