This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D1475 − 13
Standard Test Method for
Density of Liquid Coatings, Inks, and Related Products1 This standard is issued under the fixed designation D1475; the number immediately following the designation indicates the year of original origin al adoption or, in the case of revis revision, ion, the year of last revision. revision. A number in paren parenthese thesess indicates the year of last reappr reapproval. oval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Sco Scope pe 1.1 This test method covers covers the measurement measurement of density of paints, inks, varnishes, lacquers, and components thereof, other than pigments, when in fluid form. 1.2 For higher precision precision when worki working ng with nonp nonpigment igmented ed materialss (dryi material (drying ng oils, varnishes, varnishes, resins and related materials), materials), Test Method D1963 Method D1963 can can be used to determine specific gravity and, thence, density. 1.3 The values values stated in SI uni units ts are to be reg regard arded ed as the standard. The values given in parentheses are for information only. 1.3.1 Exception— The The values for density are to be stated in inch-pound units. 1.4 This standar standard d doe doess not purport purport to add addre ress ss all of the safet sa fetyy co conc ncer erns ns,, if an anyy, as asso socia ciate ted d wi with th its us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicability of regulatory limitations prior to use. A specific precaution statement is given in 8.1.1.1 in 8.1.1.1.. 2. Referenc Referenced ed Documents Documents 2.1 ASTM Standards:2 D1193 Specification for Reagent Water D1193 D1963 Test Met D1963 Method hod for Spe Specifi cificc Gra Gravit vity y of Dry Drying ing Oil Oils, s, Varn arnish ishes, es, Resi Resins, ns, and Rela Related ted Mate Materia rials ls at 25/ 25/25° 25°C C
cialty Chemica Chemicals ls (Withdrawn (Withdrawn 2009)3 E691 Practic E691 Practicee for Condu Conducting cting an Interl Interlabora aboratory tory Study to Determine the Precision of a Test Method 3. Terminology 3.1 Definitions: 3.1.1 density, n— the the mass of a unit volume of a material at a specified temperature. In this method, it is expressed as the weig we ight ht in gr grams ams pe perr mil millil lilit itre re,, or as th thee we weig ight ht in po poun unds ds avoirdupois of one U. S. gallon, of the liquid at the specified temperature; temper ature; in the absence of other temper temperature ature specification, specification, 25°C is assumed. 3.1.2 specific gravity (relative density), n— the the ratio of the mass of a unit volume of a material at a stated temperature to the mass of the same volume of distilled water at the same temperature. 4. Summ Summary ary of Test Test Method 4.1 The accurately known absolute density of distilled water at var variou iouss temp temperat erature uress (Tabl ablee 1) is us used ed to ca calib libra rate te th thee volume of a container. The weight of the paint liquid contents of the same container at the standard temperature (25°C) or at an agreed-upon temperature is then determined and density of the contents contents calc calcula ulated ted in term termss of gra grams ms per millilitre millilitre,, or pounds per gallon at the specified temperature.
3
(Withdrawn 2004)for Density, Relative Density, and API D4052 D4052 Test Test Method Gravity of Liquids by Digital Density Meter E180 Pr E180 Pract actice ice fo forr De Deter termi mini ning ng th thee Pr Preci ecisio sion n of AS ASTM TM Methods for Analysis and Testing of Industrial and Spe-
1
This test method is under the jurisdiction of ASTM Committee D01 Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of Subcommittee D01.24 Subcommittee D01.24 on on Physical Properties of Liquid Paints & Paint Materials. Current edition approved Nov. 1, 2013. Published December 2013. Originally approved in 1957. Last previous edition approved in 2012 as D1475 – 98 (2012). DOI: 10.1520/D1475-13. 2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at
[email protected]. For Annual Book of ASTM Standards volume information, refer to the standard’s Document Summary page on the ASTM website. 3 The last app approve roved d vers version ion of this historica historicall sta standa ndard rd is refe referenc renced ed on www.astm.org.
5. Significanc Significancee and Use 5.1 Densit Density y is weight per unit volume. volume. It is a key property property in the ide identi ntifica fication tion,, cha charac racteri terizati zation, on, and qua quality lity con contro troll of a widee ran wid range ge of mate materia rials. ls. Den Density sity mea measur suremen ements ts in ter terms ms of weight per gallon are commonly used to check paint quality. If the density is not within specification, there is a good chance that there was a mischarge or other serious problem. 5.2 Thi Thiss tes testt meth method od is sui suitab table le for the det determ ermina ination tion of density of paint and related products and components when in liquid form. It is particularly applicable when the fluid has too high a viscosity or when a component is too volatile for a density densit y balance determi determination nation.. 5.3 Thi Thiss test method method pro provid vides es for the max maximu imum m accu accurac racy y required for hiding power determinations. It is equally suitable for work in which less accuracy is required, by ignoring the
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D1475 − 13 TABLE 1 Absolute Density of Water, g/mL °C
Density
15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30
0.999127 0.998971 0.998772 0.998623 0.998433 0.998231 0.998020 0.997798 0.997566 0.997324 0.997072 0.996811 0.996540 0.996260 0.995972 0.995684
directions for recalibration directions recalibration and consid consideration eration of temper temperature ature differentials, and using as the container a “weight-per-gallon” cup. 5.4 Autom Automatic atic equipment equipment for measur measuring ing density is available (see Test Method D4052) D4052) from several manufacturers. manufacturers. Such apparatus has been used for resins and latices as well as for oils and an d so solv lven ents ts.. Bef Befor oree su such ch eq equi uipm pmen entt is us used ed fo forr a gi give ven n product, results must be checked very carefully. Particularly with wi th pa pain ints ts,, in inks ks,, an and d re resi sins ns,, th ther eree ar aree po poss ssib ibili ilitie tiess of gumming, fouling, and other interferences with operation. 6. Interfere Interferences nces 6.1 Highl 6.1 Highly y vi visc scou ouss ma mater terial ialss ma may y en entr trap ap air an and d gi give ve erroneous low density values. 6.2 Paint or ink liquids may be trapped trapped in the grou ground nd glass or metal joints of the pieces of apparatus and give erroneous, high density values. 7. Appar Apparatus atus 7.1 Cup or Pycnometer— Any Any metal weight-per-gallon cup or glass pycnometer may be used, provided that it may be filled readily with a viscous liquid, adjusted to exact volume, covered to exclude loss of volatile matter, and readily cleaned. NOTE 1—For materials that contain solvents that evaporate rapidly, a glass pycnometer of the weld type, with a narrow stopper and a cover should be used.
7.2 Thermometers, graduated in 0.1°C, such as are supplied with glass pycno pycnometers. meters. 7.3 Constant-Temperature Constant-Temperature Bath, held held at 25 6 0.1°C 0.1°C is desirable. 7.4 Laboratory Analytical Balance. NOTE 2—The 2—The usual weight-per-ga weight-per-gallon llon cup and simil similar ar specia specialized lized pycnometers may have filled weights that exceed the capacity of the usual labora lab orator tory y ana analyt lytica icall bala balance nce.. In suc such h cas cases, es, use of a han hangin ging g pan pan,, triple-beam balance, with scales graduated to 0.01 g has been found to provid pro videe res result ultss the mea mean n of whi which ch was consiste consistent nt wit with h the ove overal ralll precision and accuracy of the method.
7.5 Desicc or a room of Desiccato atorr and Des Desicca iccated ted Bal Balanc ance, e, or reasonably constant temperature and humidity are desirable.
8. Cali Calibrati bration on of Cup or Pycnometer Pycnometer 8.1 Determ Determine ine the volume of the contai container ner at the specifi specified ed temperature by employing the following steps: 8.1.1 8.1 .1 Clea Clean n and dry the con contain tainer er and bring bring it to con constan stantt weight wei ght.. Chr Chromi omicc acid (se (seee 8.1.1.1) 8.1.1.1) or oth other er ef effec fectiv tivee gla glass ss clean cle aner er an and d no nonr nres esid idua uall so solv lven ents ts ma may y be us used ed wi with th gl glas asss containers and solvents with metal containers. For maximum accurac accu racy y, con contin tinue ue rin rinsin sing, g, dry drying ing,, and wei weighi ghing ng unt until il the differen dif ference ce between two success successive ive weigh weighings ings does not exceed 0.001 % of the weig 0.001 weight ht of the con contain tainer er.. Fin Finger gerpri prints nts on the container will change the weight and must be avoided. Record the weight, M , in grams. 8.1.1.1 Warning—Chromic Warning—Chromic acid cleaning solution is corrosive to skin, eyes and mucous membranes and can cause severe burns. Avoid contact with eyes, skin or clothing. In making dilute solution, always add acid to water with care. Chromic acid cleaning solution is a strong oxidizer. Avoid contact with organ or ganic ic or red reduci ucing ng sub substa stance ncess as a fire could res result ults. s. See supplier’s Material Safety Data Sheet for further information. Other cleaners are much safer and may be equally effective. 8.1.2 8.1 .2 Fill the con contain tainer er with reagent reagent wat water er con confor formin ming g to Type II of Specifi Specification cation D1193 at a temp temperat erature ure som somewh ewhat at below that specified. Cap the container, leaving the overflow orifice open. Immediately remove excess overflowed water or water he water held ld in de depr pres essi sion onss by wi wipi ping ng dr dry y wi with th ab abso sorb rben entt material. Avoid occluding air bubbles in the container. 8.1. 8. 1.3 3 Br Brin ing g th thee co cont ntain ainer er an and d co cont nten ents ts to th thee sp speci ecifie fied d tempera temp eratur turee usi using ng the con constan stant-t t-temp empera eratur turee bath or roo room m if necessary. This will cause further slight flow of water from the overflow orifice due to the expansion of the water with the rise of the temperature. 8.1.4 Remove the excess overflow overflow by wiping carefully carefully with absorbent material, avoiding wicking of water out of orifice, and immediately cap the overflow tube where such has been provid pro vided. ed. Dry the out outsid sidee of the con contain tainer er,, if nec necess essary ary,, by wiping with absorbent material. Do not remove overflow that occurs subsequent to the first wiping after attainment of the desired desire d temper temperature ature (Note 3) 3). Imm Immedi ediatel ately y wei weigh gh the fille filled d container to the nearest 0.001 % of its weight (Note ( Note 4). 4). Record this weight, N , in grams. NOTE 3—Handl 3—Handling ing the con contai tainer ner wit with h bar baree han hands ds wil willl inc increa rease se the temperature and cause more overflow from the overflow orifice, and will also leave fingerprints; hence, handling only with tongs and with hands protected by clean, dry, absorbent material is recommended. NOTE 4—Imm 4—Immedi ediate ate and rap rapid id wei weighi ghing ng of the fill filled ed con contai tainer ner is recommended here to minimize loss of weight due to evaporation of the water through orifices, and from overflow subsequent to the first wiping after attainment of temperature where this overflow is not retained by a cap.
8.1.5 Calcula Calculate te the contai container ner volume as follows: follows: V 5 ~ N 2 M ! / ρ
(1 )
where: V = volum volumee of contain container, er, mL, N = wei weight ght of of contain container er and and water, water, g (8.1.4 (8.1.4)), M = wei weight ght of of dry cont contain ainer er,, g (8.1.1 (8.1.1), ), and ρ = abso absolu lute te de dens nsity ity of wa water ter at sp spec ecifi ified ed tem tempe pera ratu ture re,, g/mL (see Table (see Table 1). 1).
8.1.6 Obtain the mean of at least three determination determinations. s.
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D1475 − 13
9. Pro Procedu cedure re 9.1 Repeat the the steps in Section Section 8 8,, but do two determinations rather than three. Substitute Substitute the sample for the reagent water in Section 8 Section 8 and a suitable nonresidual solvent for the acetone or alcohol (see Note (see Note 5). 5). Record the weight of the filled container, W , and the weight of the empty container, w, in grams. NOTE 5—Trapping of paint or ink liquids in ground glass or metal joints is likely to resul resultt in high values of density that appear to increase with the viscosity viscos ity and densi density ty of the material; such errors should be minimized by firm seating of the joints. NOTE 6—Trapping of air bubbles results in low values for density. The tendency to trap air increases with increasing viscosity. Specimens should not be tested if they contain bubbles or foam. Slow stirring, standing, or the application of a vacuum may remove bubbles. If these do not work, a dilution may be necessary (see Appendix X1) X1).
9.2 Calcula Calculate te the density in grams per millilitre as follows: follows: D
m
5
~ W 2 w ! / V
(2 )
where: density y, g/mL. D = densit m
9.3 Calcula Calculate te the density in pounds per gallon as follows: D 5 ~ W 2 w ! K / V V
(3 )
where: D = densit density y, lb/gal, 8.34 3454 54 (Note 7), 7), and K = 8. volumee of contai container ner,, mL (see (see 8.1.6 8.1.6)). V = volum NOTE 7—The 7—The factor K , 8.34 8.3454, 54, is calcula calculated ted from volume-weigh volume-weightt relationship as follows: 8.345404 = [(2.54)3A × (231.00)B ]/(453.59237)C A
(2.54)3 is the conversion factor for millilitres to cubic inches. 231.00 is the conversion factor for cubic inches to gallons. C 453.59237 is the conversion factor for grams to pounds. B
10. Repor Reportt 10.1 In reporting the density, density, state the test temperature to the nearest 0.1°C, the units, and the value calculated to three places (for example, D = x.xxx lb/gal at 25°C); state the mean, the range, and the number of replicate determinations.
samples of paint ranging in density from 8.5 to 12.5 lb/gal. The results were analyzed statistically in accordance with Practice E180.. The within-laboratory coefficient of variation was found E180 to be 0.20 % relative with 25 df and the between-laboratory coefficient of variation was 0.61 % relative with 20 df. Based on these coefficients, the following criteria should be used for judging the acceptability of results at the 95 % confidence level: 11.1.1 Repeatability— Two Two results, each the mean of duplicate obtained by theifsame different daysdeterminations, should be considered suspect theyoperator differ byon more than 0.6 % relative. 11.1.2 Reproducibility— Two Two results, each the mean of duplicate determinations, obtained by operators in different laboratories should be considered suspect if they differ by more than 1.8 % relative. 11.2 Inks— A se sepa para rate te in inte terl rlab abor orato atory ry stu study dy of th this is tes testt method was carried out for inks. In this study, one operator in each of seven laboratories made three determinations on four different paste ink samples. Paste inks were chosen because their viscosities are high and they would be expected to provide a difficult test for the method. The inks represented a density range of 8.4 to 8.9 lb/gal and exhibited viscosities ranging from a very soft news black to a relatively heavy sheet-fed offset ink. The res result ultss wer weree ana analyz lyzed ed stat statisti isticall cally y in acc accord ordanc ancee wit with h Practice E691. E691. The within-laboratory standard deviation was 0.030 lb/gal and the pooled laboratory standard deviation was 0.045 0.0 45 lb/ lb/gal gal.. Bas Based ed on the these se val values ues,, the fol follow lowing ing cri criter teria ia should be used for judging the acceptability of results at the 95 % confidence level: 11.2.1 Repeatability— Two re resu sults lts ob obtai taine ned d by th thee sam samee operator should be considered suspect if they differ by more than 0.084 lb/gal (1 %). 11.2.2 Reproducibility— Two result resultss obtain obtained ed by opera operators tors in different laboratories should be considered suspect if they differ by more than 0.125 lb/gal (1.5 %). 11.3 Bias Sinc ncee th ther eree is no acc accep epte ted d Bias (Pa (Paint int and Ink Inks)— s)— Si reference material, bias cannot be determined.
11.. Pre 11 Precisi cision on and Bias 11.1 Paints— The The precision estimates are based on an interlaboratory study in which one operator in each of six different laboratories analyzed in duplicate on two different days five
12. Keyw Keywords ords 12.1 den 12.1 density sity;; pyc pycnom nomete eter; r; wei weight ght per gal gallon lon;; weig weight ht per gallon cup
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D1475 − 13 APPENDIXES (Nonmandatory Information) X1. DILUTING OF A MATERIAL MATERIAL TO TO IMPROVE AIR RELEASE
X1.1 To reduce viscosity and improve improve air release, a known weight of a material that traps air may be diluted with a known weight of a solvent or another diluent of known density. After
where: original nal materia material, l, Do = density of origi diluted measured measured in test, test, Dd1 = density diluted
careful to achieve homogeneity and air, the density blending of the diluted material is measured byrelease the technique described in this test method. The following equation may be used to calculate the density of the original material:
d2 D density sity diluen uent, t,, and W o = = den original origin al dil weight wei ght, and W d = dilu diluent ent weig weight. ht.
D
W o o
5
W o 1 W d D d1
2
W d D
(X1.1)
d2
X2. CENTRIFUGIN CENTRIFUGING G OF MATERIAL TO REMOVE EXCESS AIR
X2.1 To red X2.1 reduce uce the var variati iation on in the density density method, method, air is remove rem oved d fro from m the spe specime cimen n by cen centri trifug fuging ing the mate material rial,, resulti res ulting ng in gre greater ater hom homoge ogenei neity ty bet betwee ween n rep replica licates tes.. Thi Thiss
X2.3.2 Tur Turn n on the centri centrifuge fuge and set the speed control to 2/3 power to attain a speed of 2700 to 3000 r/min.
greatly improves and repeatability and results in slightly higher reproducibility density readings.
applying the brake as needed. X2.3.4 Pour off off the top foam layer. layer.
X2.2 Appar Apparatus atus X2.2.1 Centrifuge, capable of a maximum of 4000 r/min ,
X2.3.5 X2. 3.5 Tr Trans ansfer fer the spe specime cimen n to a cali calibra brated ted den density sity cup and follow the procedure under Section 9.
X2.2.2 Standard Density Cup,
X2.4 Pr Precis ecision ion and Bias
X2.2.3 Thermometer.
X2.4.1 An inte X2.4.1 interla rlabor borato atory ry stu study dy in one com compan pany y sho showed wed that the centrif centrifuge uge procedure procedure result resulted ed in a 2-fol 2-fold d impro improvemen vementt in repea repeatability tability and repro reproducib ducibility ility,, as well as better accuracy. accuracy. X2.4.1.1 Repeatability— Two Two results obtained by the same operator should be considered suspect if they differ by more than 0.0054 g/mL (0.045 lb/gal). X2.4.1.2 Reproducibility— Two result resultss obtain obtained ed by operators in different laboratories should be considered suspect if
4
X2.3 Procedur Proceduree X2.3.1 X2. 3.1 Fill the cen centrif trifuge uge tube to the top (approxi (approximate mately ly 150 % of the density cup volume), adjust to the recommended temperature of 25°C 6 1. Place the tube in the centrifuge.
4
X2.3.3 Contin Continue ue to run for 15 to 20 s, stop the centrifuge, centrifuge,
The centrifuge used in this study was a Dynac II.
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