1、Designation: D 365 01 (Reapproved 2005)Standard Guide forSoluble Nitrocellulose Base Solutions1This standard is issued under the fixed designation D 365; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、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 This guide covers the testing of soluble nitrocellulosebase solutions that are made by dispersing various kinds andconcentrations of s
3、oluble nitrocellulose (cellulose nitrate) invarious solvent mixtures.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use.
4、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 use. For specific hazardstatements see Section 11.2. Referenced Documents2.1 ASTM Standards:2D 301 Test Methods for Soluble C
5、ellulose NitrateD 333 Test Methods for Clear and Pigmented LacquersD 1193 Specification for Reagent WaterD 1200 Test Method for Viscosity by Ford Viscosity CupE 300 Practice for Sampling Industrial Chemicals3. Significance and Use3.1 Since the desired specifications and compositions ofsoluble nitroc
6、ellulose base solutions vary greatly, these meth-ods are used to establish whether limits that shall be as agreedupon between the producer and the user have been met.4. Sampling4.1 Select the sampling method from those listed in PracticeE 300.CONSISTENCY (VISCOSITY)5. Consistency Tests5.1 For Consis
7、tencies from 3 to 500 sDetermine theconsistency by falling-ball consistency test described in TestMethods D 301 for those solutions having a consistency from3 to 500 s when tested in that apparatus.5.2 For Consistencies Less than 3 sDetermine the con-sistency by Test Method D 1200 for those solution
8、s having aconsistency of less than 3 s when tested in the falling-ballapparatus referred to in 5.1.5.3 For Consistencies over 500 sDetermine the consis-tency using the apparatus and procedure described in Sections6 and 7 for those solutions having a consistency greater than500 s when tested in the f
9、alling-ball apparatus referred to in5.1.6. Apparatus6.1 The consistency test apparatus, shown in Fig. 1, shallconsist of the following:6.1.1 Glass Tube (preferably heat-resistant glass),350 61.5 mm (2 6132 in.) in inside diameter and 255 mm (10 in.)in length, with marks 177 6 1mm(56116 in.) apart, t
10、heupper one being 75 mm (3 in.) from the top of the tube.NOTE 1The steel ball can be removed (in order to leave the samematerial in the tube for a check run) by removing the lower stopper.However, a small air bubble is usually introduced in this way. It ispreferable to invert the tube, removing the
11、guide to get the ball out. It isoften necessary to put a few drops of solvent in the guide lip to loosen itfrom the tube on account of the solution drying at the edge of the tube.When the latter method is used for removing the ball, a larger bubbletraverses the tube than when the former method is us
12、ed, but a large bubblemoves sufficiently fast, even in a very viscous solution, to escape at the topin a few minutes, whereas small bubbles take hours to escape.6.1.2 Steel Ball, 15.88 6 0.02 mm (0.625 6 0.001 in.) indiameter, and weighing 16.536 6 0.10 g.6.1.3 Aluminum Guide Cone of light gage alum
13、inum (ap-proximately 0.5 mm (0.02 in.) in thickness) as shown in Fig. 1.The orifice of the guide cone shall be 22 mm (78 in.) in1This guide is under the jurisdiction of ASTM Committee D01 on Paint andRelated Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.55
14、 on Factory Applied Coatings on Preformed Products.Current edition approved May 15, 2005. Published August 2005. Originallyapproved in 1933. Last previous edition approved in 2001 as D 365 01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at ser
15、viceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Borosilicate glass is satisfactory for this purpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.d
16、iameter, the conical portion 25 mm (1 in.) in height, thecylindrical portion 12.7 mm (12 in.) in height, and the outsidediameter shall be slightly under 50 mm (2 in.) so as to fitsnugly into the viscosity tube.6.1.4 Stoppers, made preferably of rubber and covered withtin foil.7. Procedure7.1 Fill th
17、e tube in any convenient manner whereby bubblesdo not form and no appreciable amount of solvent is lost. Onemethod is to immerse the lower end of the open tube in thesolution and to apply suction at the upper end of the tube. Inthis manner the tube can be filled in from 5 to 10 s without theintroduc
18、tion of air bubbles or an appreciable loss of solvent.Close the bottom of the tube with a stopper covered with tinfoil. Push the aluminum guide cone slowly into the top of thetube and insert a stopper covered with tin foil into the top of theguide.7.2 Bring the tube and its contents to a temperature
19、 of 25 60.1C by placing in a suitable bath. Allow at least 30 min forthe solution to reach temperature equilibrium. For accuratemeasurements keep the tube during the determination either ina thermostat or suspended within a considerably larger cylinderof water at the specified temperature.7.3 Remove
20、 the upper stopper only long enough to place theball in the center of the tube; this can be done convenientlywith crucible tongs. The principal value of the guide cone is toretard the ball sufficiently at the start of its fall so that thesolution will close over the ball and not leave on the top of
21、theball a large “trailer bubble.” If the guide is not used a big trailerbubble usually accompanies the ball, retarding its fall and, ifthe bubble is off center on the ball, pulling the latter away fromthe center of the tube.7.4 Measure the time of fall in seconds from the instant thebottom of the ba
22、ll is level with the upper reference mark on thetube until it reaches the lower mark on the tube.NONVOLATILE MATTER8. Procedure8.1 Determine the percent of nonvolatile matter in accor-dance with the procedure described in the Nonvolatile Mattersection of Test Methods D 333.APPEARANCE OF SOLUTION9. P
23、rocedure9.1 Compare the appearance of the soluble nitrocellulosebase solution with a reference standard agreed upon betweenthe purchaser and the seller (both the reference standard andsample solutions shall be thoroughly agitated before makingobservations) in similar bottles for turbidity, hair, gra
24、in, andinsoluble matter.DEPTH OF COLOR10. Apparatus10.1 The apparatus used for the preparation of the colorstandards and for the depth of color determinations shallconsist of the following:10.1.1 LightSource of transmitted light.NOTE 2Not absolutely necessary but will increase accuracy and bemore co
25、nvenient.10.1.2 Bottles, three dozen 60 m (2-oz L) screw-cap, square,glass.10.1.3 Flasks, several, 1-L, volumetric.10.1.4 Burets, two, 50-mL.10.1.5 Analytical Balance.10.1.6 ColorimeterDubosq colorimeter (see Note 2).10.1.7 Color GlassYellow glass about 25 mm square and10 mm thick.411. Reagents and
26、Materials11.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.5Other
27、grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.11.2 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type III
28、 of Specification D 1193.4The sole source of supply of color glass, signal yellow No. 330, known to thecommittee at this time is Corning Glass Works, Corning, NY. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive c
29、areful consideration at a meeting of theresponsible technical committee,1which you may attend.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Stan
30、dards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 1 Apparatus for Consistency (Viscosity) Test of SolutionsHaving Consistencies over 500 sD 365 01 (2005)211.3 Potassium
31、 Chloroplatinate,(K2PtCl6). Warning: Thismaterial is hazardous. Carefully review Material Safety DataSheets supplied by manufacturers for handling and first aidinstruction.11.4 Cobalt Chloride (CoCl26H2O). (WarningSee 11.3.)11.5 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl). (
32、WarningSee 11.3.)11.6 Caramel (sugar coloring).11.7 Phenol.(WarningSee 11.3.)12. Preparation of Color Standards12.1 Platinum-Cobalt Color Standards Prepare theplatinum-cobalt color standards as follows: Weigh out on ananalytical balance exactly 1.245 g of K2PtCl6and 1.000 g ofcrystallized cobalt chl
33、oride (CoCl26H2O). Dissolve in distilledwater, add 100 mL of HCl (sp gr 1.19), and dilute to 1000 mLwith distilled water. This solution is color standard No. 10.6Prepare color standards Nos. 1 to 10, inclusive, by accuratelymeasuring from burets directly into the square 2-oz (60-mL)bottles the quant
34、ities shown in Table 1 of the No. 10 colorstandard and distilled water. After preparation of the colorstandards seal the bottles with corks and paraffin before puttingon the screw caps. The platinum-cobalt color standards arepermanent for approximately six months. Make the colorstandards from No. 12
35、 to No. 500, inclusive, from a caramelsolution, but the color is based on the platinum-cobalt colorstandard.12.2 Caramel Color StandardsPrepare the caramel colorstandards as follows: Dilute caramel (sugar coloring) in theratio of about 1 mL of caramel to 100 mL of distilled water ina glass vessel. A
36、dd 0.5 % phenol and agitate thoroughly.Adjust the concentration of this solution so that when it isdiluted in the ratio of 1 mL of solution to 49 mL of distilledwater, to which has been added 0.5 % phenol, the solution willmatch color No. 10 of the platinum-cobalt color standard. Thiscaramel solutio
37、n before dilution is color No. 500 (Note 3).Prepare color standards No. 12 to No. 500, inclusive, byaccurately measuring from burets directly into the square 2-oz(60-mL) bottles the quantities shown in Table 2 of color No.500 caramel standard and distilled water to which has beenadded 0.5 % phenol.
38、After preparation of the color standards,seal the bottles with corks and paraffin before putting on thescrew caps. All of the caramel color standards are permanentfor approximately one month but should be checked semi-monthly if frequently used.NOTE 3It is more convenient to check the caramel color
39、standard No.500 against a colored glass that has been previously standardized againstthe platinum-cobalt color standard; a piece of signal yellow glass (see10.1.7) about 25 mm square by 10 mm thick may be standardized and usedas a check on the caramel solution. This must be done by use of acolorimet
40、er.13. Procedure13.1 Fill a square 60-mL (2-oz) glass bottle with thematerial to be tested and match this against one of the colorstandards using either direct daylight or indirect artificialtransmitted light, the latter being preferred. The number of thecolor standard matched is the depth of color
41、of the material.14. Precision and Bias14.1 The precision and bias of these test methods is asdescribed for each of the separate methods cited if available.15. Keywords15.1 appearance; consistency testing; depth of color; non-volatile matter; soluble nitrocellulose base solutions6This solution has an
42、 assigned value of 500 on the Hazen color scale (seeAmerican Chemical Journal, Vol XIV, p. 300).TABLE 1 Platinum-Cobalt Color StandardsPlatinum-CobaltColor StandardsQuantity ofNo. 10 ColorStandard, mLQuantity ofDistilledWater, mLNo. 1 5 45No. 2 10 40No. 3 15 35No. 4 20 30No. 5 25 25No. 6 30 20No. 7
43、35 15No. 8 40 10No. 9 45 5No. 10 50 0TABLE 2 Caramel Color StandardsCaramel ColorStandardsQuantity ofNo. 500Caramel ColorStandard, mLQuantity ofDistilledWater plusPhenol, mLNo. 12 1.2 48.8No. 15 1.5 48.5No. 20 2.0 48.0No. 25 2.5 47.5No. 30 3.0 47.0No. 35 3.5 46.5No. 40 4.0 46.0No. 45 4.5 45.5No. 50
44、5.0 45.0No. 60 6.0 44.0No. 70 7.0 43.0No. 75 7.5 42.5No. 80 8.0 42.0No. 90 9.0 41.0No. 100 10.0 40.0No. 125 12.5 37.5No. 150 15.0 35.0No. 175 17.5 32.5No. 200 20.0 30.0No. 250 25.0 25.0No. 300 30.0 20.0No. 350 35.0 15.0No. 400 40.0 10.0No. 450 45.0 5.0No. 500 50.0 0.0D 365 01 (2005)3ASTM Internation
45、al 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, and the riskof infringement of such rights, are entirely their
46、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 revision of this standard or for additional standardsand should be
47、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 you shouldmake your views known to the ASTM Committee on Standards,
48、 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).D 365 01 (2005)4
