1、Designation: F3139 15Standard Test Method forAnalysis of Tin-Based Solder Alloys for Minor and TraceElements Using Inductively Coupled Plasma AtomicEmission Spectrometry1This standard is issued under the fixed designation F3139; the number immediately following the designation indicates the year ofo
2、riginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers procedures for the analysis oftin-ba
3、sed solder alloys for minor and trace elements usinginductively-coupled plasma atomic emission spectrometry(ICP-AES) instrumentation.1.2 These test procedures were validated for the analytesand mass fractions listed below.Element Validated Mass FractionRange, mg/kgLead 115 to 965Cadmium 25 to 60Merc
4、ury 5 to 530Antimony 85 to 1330Bismuth 80 to 210Arsenic 95 to 360Silver 4000 to 42100Cobalt 0.5 to 60Iron 15to115Chromium 0.5 to 1.5Copper 3000 to 30600Indium 25 to 115Nickel 5 to 150Phosphorus 10 to 110Selenium 1 to 30Zinc 2 to 160Aluminum 1 to 31.3 The procedures appear in the following order:Proc
5、edure SectionInternal Standardization 8Calibration Solution Preparations 9Preparation of Sample and Validation Solutions 10Calibration 11Analysis Procedure 121.4 The values stated in SI units are to be regarded as thestandard. Any other values are for information only.1.5 This standard does not purp
6、ort 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 use.2. Referenced Documents2.1 ASTM Standards:2D11
7、29 Terminology Relating to WaterE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE416 Practice for Planning and Safe Operation of a Spec-trochemical Laboratory (Withdrawn 2005)3E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE14
8、79 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission Spectrometers3. Terminology3.1 DefinitionsFor definitions of other terms used in thistest method, refer to Terminology D1129.3.2 Acronyms:3.2.1 ACS, nAmerican Chemical Society3.2.2 ICP-AES, ninductively-coupled plas
9、ma atomicemission spectrometry3.2.3 PE, npolyethylene3.2.4 SI, nLe Systme International dUnits, Interna-tional System of Units3.3 Definitions of Terms Specific to This Standard:3.3.1 calibration blank, na volume of water containingthe same acid matrix as found in the calibration standards.3.3.2 cali
10、bration standards, na series of known standardsolutions used to calibrate an instrument.3.3.3 check standard, nstandard used to verify properinstrument calibration.1This test method is under the jurisdiction of ASTM Committee F40 onDeclarable Substances in Materials and is the direct responsibility
11、of SubcommitteeF40.01 on Test Methods.Current edition approved May 1, 2015. Published July 2015. DOI: 10.1520/F3139-152For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer t
12、o the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.3.4 instrument linear range, nrange where i
13、nstrumentresponse and accuracy remain within typically 5 to 10 % ofknown values.3.3.5 internal standard, npure element(s) added in knownamount(s) to a solution to be used to improve instrumentaccuracy.3.3.6 reference material solution, nsolution standard withknown certified mass fraction(s), typical
14、ly commercially avail-able.3.3.7 sample introduction system, nplasma torch, mixingchamber and nebulizer used to deliver solutions to the plasmafor analysis.3.3.8 validation sample, na solder alloy sample that hasbeen certified or well characterized for mass fractions ofanalytes present, and can be u
15、sed to validate the method.4. Significance and Use4.1 Tin-based solder alloys are commonly used to manufac-ture electrical and electronic goods. The elements lead,cadmium, mercury, antimony and bismuth are often declarablesubstances in solder materials. This test method provides ameans of determinin
16、g the listed declarable substances, as wellas other minor and trace constituents, in tin-based solder alloys.4.2 Two methods of dissolving tin-based solder alloys aregiven in this standard. The first method uses open-vesselhydrofluoric and nitric acid room temperature digestions; thesecond method em
17、ploys closed-vessel nitric and hydrofluoricacid microwave digestions, both for use only with ICP-AESinstruments equipped with a hydrofluoric acid resistant sampleintroduction system.4.3 The method of preparing calibration solutions uses 1000mg/kg single element reference material solutions, and uses
18、matching concentrated acids for both the calibration solutionsand the sample solutions.4.4 This test method is intended for use by laboratoriesexperienced with the set-up, calibration and analysis ofsamples using ICP-AES.5. Reagents5.1 Purity of ReagentsReagent grade chemicals, at aminimum, shall be
19、 used in all tests. Unless otherwise indicated,all reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades equiva-lent or better than the ACS grade reagents may also be used.5.2 Purit
20、y of WaterUnless otherwise indicated, referencesto water shall be understood to mean high purity water, thatwhen produced, measures at minimum 18 Megohm cm-1resistivity.5.3 Concentrated AcidsWhen acids are specified by nameor chemical formula only, it should be understood that concen-trated reagents
21、 of the following mass fractions are intended:Concentrated AcidNominal MassFractionHydrofluoric acid, HF 48 %Nitric acid, HNO369 %5.4 Single Element Reference Material SolutionsAllsingle element solutions used in this method must haveassigned mass fraction values in mg/kg units as opposed tomg/L uni
22、ts. It is possible to derive mg/kg values from mg/Lassigned values through determination of standard solutiondensity and subsequent calculation of mg/kg unit values.5.4.1 The method of preparing calibration solutions uses1000 mg/kg single element reference material solutions of Pb,Cd, Hg, Sb, Bi, As
23、, Ag, Co, Fe, Cr, Cu, In, Ni, P, Se, Zn, Al,Ge, and Tl. A single element reference material solution of Scat 1000 mg/kg is required for use as an internal standard.5.4.2 It is not important that the assigned value of thereference material solutions be exactly 1000 mg/kg; forexample, the assigned val
24、ue may be 1001 mg/kg or 997 mg/kg.6. Equipment6.1 Inductively Coupled Plasma-Atomic Emission Spec-trometry System (ICP-AES)Many makes and models ofICP-AES instruments are available on the market. See PracticeE1479 for a general description of ICP-AES instrumentation.The specific instrumentation used
25、 is not as important as itsperformance with regard to precision and sensitivity. However,a few important considerations for successful method perfor-mance are given below:6.1.1 Sample Introduction SystemMeasurement ofsamples prepared using hydrofluoric acid (HF) requires that thesample introduction
26、system must be designed specifically tocome in contact with HF. Glass sample introduction systemsare not compatible with HF, as glass is dissolved (etched) bythe acid. HF contact causes excessive wear of glass parts andcontamination of samples, thus having a negative impact on theequipment as well a
27、s results. Consult with the instrumentmanufacturer before using solutions containing HF.6.1.2 NebulizerAnalysis of samples prepared using HFrequires that the nebulizer, as part of the sample introductionsystem, must be compatible with HF. In addition, this methodrequires analysis of solutions with r
28、elatively high solidscontent on the order of 0.5 % by mass (5000 mg/kg). Thenebulizer should be chosen to accommodate free flow ofhigh-solids solutions such that the nebulizer does not clogduring the procedure, thus allowing consistent sample intro-duction.6.1.3 Facility DesignA general description
29、of design con-siderations for a spectrochemical laboratory can be found inPractice E416. Temperature control within the laboratoryhousing the ICP-AES system, and consistent power supply tothe instrument are two of the most important considerations.ICP-AES equipment tends to produce a significant amo
30、unt ofheat while in operation and variation in room temperature can4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemica
31、ls, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.F3139 152have a significant impact on the stability of instrument mea-surements. Sufficient equipment warm-up period and subse-quent stabilization of
32、room temperature may be necessary toproduce consistent measurements. Variations in power sup-plied to the instrument can likewise have an impact on thestability of instrument measurements, so stabilization of thepower input may also be necessary to produce consistentmeasurements.6.2 Analytical Balan
33、ceAbalance with minimum readabil-ity of 0.0001 g for loads up to 150 g is required for successfulperformance of this method.6.3 Microwave Digestion EquipmentModern laboratorymicrowave equipment, including pressure vessels, provide heatand pressure to digest difficult samples without potential loss o
34、fanalytes common to open hotplate digestions. Closed-vesselmicrowave digestion can help prevent possible loss of volatileelements, such as mercury, during sample preparation. Useonly microwave equipment designed specifically for laboratoryuse.7. Hazards7.1 Hydrofluoric acid and hydrofluoric acid fum
35、es can posesignificant risk to the operator. Proper handling should beobserved at all times, including the use of laboratory fumehoods, and laboratory coats, polymer gloves and protectiveeyewear. Carefully handle all solutions. Be sure to let micro-wave vessels cool for a sufficient amount of time b
36、eforeopening. Be sure to use only HF resistant sample introductioncomponents so as not to cause damage to glass parts. Alwaysmaintain the capability to flush skin with water for at least 5min in case of skin contact with HF; keep calcium gluconate orequivalent in the laboratory to neutralize contact
37、 with HF. Seekappropriate emergency medical help after contact with HF orHF fumes for unknown or extended periods of time.8. Internal Standardization8.1 The internal standard procedure requires that every testsolution have the same mass fraction of an internal standardelement that is not present in
38、the original specimen. Specimento specimen changes in the emission intensity of the internalstandard element can be used to correct for variations in the testspecimen introduction efficiency, which is dependent on thephysical properties of the test specimen (such as dissolvedsolids content, acid mas
39、s fraction, etc).8.2 Internal Standard SolutionWeigh approximately 5 g(to the nearest 10 mg) of 1000 mg/kg Sc reference materialsolution into a 100 mL polyethylene bottle and dilute to 100 gwith 5 % v/v HNO3. Prepare fresh at least monthly. The samebatch of internal standard solution should be used
40、for allblanks, calibrations standards, validation samples, and un-known samples within an analysis.9. Calibration Solution Preparations9.1 Preparation of Calibration SolutionsSample Prepara-tion Method 1, Section 10.1:9.1.1 Calibration BlankPrepare a calibration blank bymaking a 10 % v/v HNO3/10 % v
41、/v HF solution, and adding2.0 g 6 20 mg (weighed to the nearest 10 mg) of 50 mg/kg Scinternal standard solution per 100 g final weight of blanksolution. The Sc internal standard will be at the same massfraction as in the calibration standards and samples (1.0 mg/kgSc).9.1.2 Calibration Standards2 mg
42、/kg and 10 mg/kgWeigh 0.2 g 6 2mgand1g6 10 mg (to the nearest 1 mg),respectively, of each of the single element 1000 mg/kg refer-ence material solutions into 100 mL polyethylene bottles.Dilute each with approximately 50 g of 10 % v/v HNO3/10 %v/v HF, and add 2.0 6 0.2 g (weighed to the nearest 10 mg
43、) of50 mg/kg Sc internal standard solution. Dilute to final weightof 100 g 6 1.0 g (weighed to the nearest 100 mg) with 10 %v/vHNO3/10 % v/v HF.9.1.3 Check StandardsPrepare at least one instrumentcheck standard in the same manner as the calibration standards,such that the element mass fractions in t
44、he check standards aresimilar to the element mass fractions in the test samples.9.1.4 Verify that the internal standard element is stable insolution by visually examining for cloudiness or precipitate.9.2 Preparation of Calibration SolutionsSample Prepara-tion Method 2, Section 10.2:9.2.1 Prepare ca
45、libration standards as directed in 9.1, usinga 7 % v/v HNO3/7 % v/v HF acid mixture, instead of the 10 %v/v HNO3/10 % v/v HF solution.10. Preparation of Sample and Validation Solutions10.1 Method 1Open Vessel DigestionFor each sampleand validation sample, weigh out 0.5 g 6 10 mg (to the nearest1 mg)
46、 and place into 60 mL polyethylene bottles. This sampleweight is defined as SW1. To digest, add 5 mL H2O, followedby the slow addition of 5 mL concentrated HF. Add 5 mLconcentrated HNO3in 0.2 mL increments to reduce volatilityof the reaction. Most samples will dissolve immediately orwithin 5 to 10 m
47、in.Add approximately 20 g H2O to sample andmix. Add 1.0 g 6 10 mg (weighed to the nearest 10 mg) of 50mg/kg Sc internal standard solution (prepared from 1000mg/kg Sc reference material solution), and dilute sample tofinal weight of 50 6 0.5 g (weighed to the nearest 10 mg) withH2O. The final weight
48、of the diluted sample is defined as FW1.Prepare a blank solution in the same manner. Verify thestability of the internal standard as described in 9.1.4.NOTE 1Warning: Take precautions to protect lab personnel from theharmful effects of contact with HF. Treat HF exposure immediately; see7.1 for addit
49、ional information.10.2 Method 2Closed-Vessel Microwave DigestionForeach sample and validation sample, weigh out 0.5 g 6 10 mg(to the nearest 1 mg) and place into a high-pressure microwavevessel. This sample weight is defined as SW1.Add dropwise 10mL of 1:1:1 H2O/conc. HNO3/conc. HF. Caution must be usedas the reaction is quite vigorous and exothermic. Close vesseland digest in laboratory microwave oven according to thefollowing program:Heating Program: Ramp to TemperatureMax Power = 800 WPower = 100 %Power Ramp = 10 minMaximum Pressure = 800 psi (
