1、Designation:D 1064 97Standard Test Methods forIron in Rosin Tall Oil Fatty Acids and Other RelatedProducts1This standard is issued under the fixed designation D 1064;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last re
2、vision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon(e)indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1.Scope1.1 These test methods cover colorimetric procedures
3、 forthe determination of iron in rosin tall oil fatty acids and otherrelated products.Both spectrophotometric and visual methodsare covered.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 e
4、stablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Significance and Use2.1 Iron is a possible contaminant in naval stores products,being introduced into these products during their productionfrom various raw material sources.Gu
5、m rosin in particular isprone to iron contamination as the equipment used for itscollection and processing is often made from iron containingmetals.2.2 Iron is a troublesome contaminant in rosin and fattyacids,as even trace quantities will catalyze the oxidation and asubsequent darkening of these pr
6、oducts.2.3 The test methods described in this standard were devel-oped many years ago and to a large extent have been replacedby modern instrumental methods such as atomic absorbanceand inductively coupled plasma spectroscopies.The test meth-ods described in this standard are subject to interference
7、s fromother species in the sample being tested.However,the testmethods described here are acceptable if approximate or trendvalues are required and if appropriate analytical instrumenta-tion is not available.3.Reagents3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless oth
8、erwise 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.2Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high pur
9、ity to permit its use without lessening theaccuracy of the determination.3.2 Unless otherwise indicated,references to water shall beunderstood to mean deionized or distilled water.SPECTROPHOTOMETRIC METHOD4.Summary of Test Method4.1 Ferrous iron,in a dilute hydrochloric acid solution,forms a red-col
10、ored complex with 1,10-phenanthroline.Theintensity of the color is measured at approximately 505 nm bymeans of a spectrophotometer.5.Apparatus5.1 PhotometerAny spectrophotometer or filter photom-eter that will measure accurately the transmittance of thesolutions in the range from 500 to 520 nm.5.2 D
11、ishes,high-silica glass,3silica,or porcelain,50 and100-mL capacity.NOTE1Platinum or platinum-rhodium dishes are not recommendedas they sometimes cause a color interference with the phenanthrolinereagent.5.3 Watch Glasses,to cover the dishes described in 5.2.5.4 PipetsOne 100-mL,two 10-mL,three 5-mL,
12、and two2-mL pipets.5.5 Measuring Pipet,Mohr-type,10-mL.5.6 Volumetric Flasks,1-L and 50-mL capacities.5.7 Absorption Cells,having a capacity of at least 25 mL.1These test methods are under the jurisdiction ofASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and are the direc
13、t responsibilityof Subcommittee D01.34 on Naval Stores.Current edition approved June 10,1997.Published September 1997.Originallypublished as D 1064 49.Last previous edition D 1064 93.2Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on
14、 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.Pharmacopoeial Convention,Inc.(USPC),Rockville,MD.3The sole source of supply of the high-silica gla
15、ss known to the committee atthis time is Vycor.If you are aware of alternative suppliers,please provide thisinformation to ASTM Headquarters.Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.1AMERICAN SOCIETY FOR TESTING AND M
16、ATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMSmaller cells may be used when the color is developed in aflask or beaker.6.Reagents6.1 Hydrochloric Acid(1+19)Dilute 1 volume of A.C.S.grade HCl(sp gr 1.18)with 19 volumes of water.6.2 Iron Solution,Standard(1 mL 5 0.1 mg Fe)Dissolve0.1000 g of pure iron wire(99.85%iron)in 10 mL of H2SO4(1+9)and 3 mL of HNO3(sp gr 1.42).Dilute with water to 1L in a volumetric flask.6.3 Iron Solut