1、Designation: D7458 14Standard Test Method forDetermination of Beryllium in Soil, Rock, Sediment, and FlyAsh Using Ammonium Bifluoride Extraction andFluorescence Detection1This standard is issued under the fixed designation D7458; the number immediately following the designation indicates the year of
2、original 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. Scope*1.1 This test method is intended for use in the determinationo
3、f beryllium in samples of soil, rock, sediment, and fly ash.This test method can be used for purposes such as environ-mental remediation projects where beryllium is a contaminantof concern. It is also useful for characterization of levels ofberyllium in soil at sites where beryllium is in mining orm
4、anufacturing applications, and for determination of back-ground levels of beryllium in soil.1.2 This test method assumes that samples of soil, rock,sediment, or fly ash are collected using appropriate andapplicable ASTM International standard practices.1.3 This test method includes a procedure for e
5、xtraction(dissolution) of beryllium in dilute ammonium bifluoride,followed by analysis of aliquots of the extract solution using aberyllium-specific fluorescent dye.1.4 No detailed operating instructions are provided becauseof differences among various makes and models of suitablefluorometric instru
6、ments. Instead, the analyst shall follow theinstructions provided by the manufacturer of the particularinstrument. This test method does not address comparativeaccuracy of different devices or the precision between instru-ments of the same make and model.1.5 The values stated in SI units are to be r
7、egarded asstandard. No other units of measurement are included in thisstandard.1.6 All observed and calculated values shall conform to theguidelines for significant digits and rounding established inPractice D6026.1.6.1 The procedures used to specify how data are collected/recorded, or calculated, i
8、n this standard are regarded as theindustry standard. In addition, they are representative of thesignificant digits that generally should be retained. The proce-dures used do not consider material variation, purpose forobtaining the data, special purpose studies, or any consider-ations for the users
9、 objectives; and it is common practice toincrease or reduce significant digits of reported data to becommensurate with these considerations. It is beyond the scopeof this standard to consider significant digits used in analyticalmethods for engineering design.1.7 This test method contains notes that
10、 are explanatory andnot part of mandatory requirements of the standard.1.8 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 establish appro-priate safety and health practices and determine th
11、e applica-bility of regulatory limitations prior to use. Specific hazardsassociated with performance of this test method are describedin Section 9.2. Referenced Documents2.1 ASTM Standards:2D653 Terminology Relating to Soil, Rock, and ContainedFluidsD1193 Specification for Reagent WaterD3740 Practic
12、e for Minimum Requirements for AgenciesEngaged in Testing and/or Inspection of Soil and Rock asUsed in Engineering Design and ConstructionD4840 Guide for Sample Chain-of-Custody ProceduresD5730 Guide for Site Characterization for EnvironmentalPurposes With Emphasis on Soil, Rock, the Vadose Zoneand
13、Groundwater (Withdrawn 2013)3D6026 Practice for Using Significant Digits in GeotechnicalDataD7202 Test Method for Determination of Beryllium in theWorkplace by Extraction and Optical Fluorescence Detec-tion1This test method is under the jurisdiction ofASTM Committee D18 on Soil andRock and is the di
14、rect responsibility of Subcommittee D18.01 on Surface andSubsurface Characterization.Current edition approved May 1, 2014. Published June 2014. Originallyapproved in 2008. Last previous edition approved in 2008 as D7458 - 08. DOI:10.1520/D7458-14.2For referenced ASTM standards, visit the ASTM websit
15、e, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section
16、appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precisio
17、n of a Test MethodE882 Guide for Accountability and Quality Control in theChemical Analysis Laboratory2.2 Other Standards:ISO 594-2 Conical Fittings with a 6 % (Luer) Taper forSyringes, Needles and Certain Other MedicalEquipmentPart 2: Lock FittingsEN ISO 8655-2 Piston-Operated Volumetric PipettesPa
18、rt2: Piston Pipettes43. Terminology3.1 DefinitionsFor definitions of common technical termsin this standard, see Terminology D653.4. Summary of Test Method4.1 This standard test method is used to determine theberyllium content of soil, rock, sediment, and fly ash. Samplesare collected in the field u
19、sing procedures described in ASTMInternational standards (see Guide D5730 for listings ofappropriate sample collection standards).A0.5-gram aliquot isextracted using 3 % ammonium bifluoride solution heated at90C for 40 hours. The presence of active fluoride ions (HF bydissociation of ammonium bifluo
20、ride in acidic medium) en-ables dissolution of refractory forms of beryllium, includingsilicates, borosilicates, and oxides. The extraction solutionproduced from each sample is then filtered and an aliquot ofthis extract is added to a pH-adjusted detection solution whichcontains a beryllium-specific
21、 fluorescence reagent. The fluo-rescence of this final solution is then measured on a calibratedfluorometer to quantify the amount of beryllium in the sample.This standard test method is adapted from Test Method D7202.4.2 The limit of quantification of this test method is 0.013milligrams beryllium p
22、er kilogram of sample, based on a0.5-gram sample (1).55. Significance and Use5.1 Exposure to beryllium can cause a potentially fataldisease, and occupational exposure limits for beryllium in airand on surfaces have been established to reduce exposure risksto potentially affected workers (2, 3). Meas
23、urement of beryl-lium in matrices such as soil, rock, sediment, and fly ash isimportant in environmental remediation projects involvingberyllium contamination (4) and for establishment of back-ground levels of beryllium at sites where anthropogenicberyllium may have been used (2). Sampling and analy
24、ticalmethods for beryllium are needed in order to meet thechallenges relating to exposure assessment and risk reduction.Sampling and analysis methods, such as the procedure de-scribed in this test method, are desired in order to facilitatemeasurements of beryllium that can be used as a basis formana
25、gement of remediation projects and protection of humanhealth.5.2 This test method can be used for purposes such asenvironmental remediation projects where beryllium is a con-taminant of concern. It is also useful for characterization oflevels of beryllium in soil at sites where beryllium is in minin
26、gor manufacturing applications, and for determination of back-ground levels of beryllium in soil.NOTE 1The quality of the result produced by this standard isdependent on the competence of the personnel performing it, and thesuitability of the equipment and facilities used. Agencies that meet thecrit
27、eria of Practice D3740 are generally considered capable of competentand objective testing, sampling, inspection, and so forth. Users of thisstandard are cautioned that compliance with Practice D3740 does not initself assure reliable results. Reliable results depend on many factors;Practice D3740 pro
28、vides a means of evaluating some of those factors.6. Interferences6.1 This test method is highly specific for beryllium. Othersolvated metal ions are either bound by ethylenediaminetet-raacetic acid (EDTA) in the detection solution, or they precipi-tate out due to the high alkalinity of the detectio
29、n solution. Thefluorophore used for detection is highly specific for theberyllium divalent cation (Be+2).6.2 If iron or titanium are present in high excess in thesample (typically above 7 %), the resulting measurementsolution may appear golden-yellow. In this case the solution isleft for two hours o
30、r more for the iron or titanium (or both) toprecipitate. The solution is then re-filtered using the sameprocedure as for filtering the dissolution solution (after thedissolution step), prior to fluorescence measurement.7. Apparatus7.1 Sampling EquipmentUse sampling apparatus appro-priate for the typ
31、e of media being collected (for example, soil,rock, sediment, fly ash) and its location (for example, surface,subsurface, vadose zone). Guidance on selection of appropriatesampling apparatus is found in the ASTM International stan-dards referenced in Guide D5730.7.2 Instrumentation:7.2.1 Ultraviolet
32、/Visible (UV/Vis) Fluorometer, with irradi-ance excitation lamp or light-emitting diode (excitation = 380nm) and time-integrating visible detector (400700 nm, max 475 nm).7.2.2 Laboratory Balance, capable of measuring to thenearest 0.1 mg.7.2.3 Laboratory Oven, capable of maintaining a tempera-ture
33、of 90 6 2C.7.3 Laboratory Supplies:7.3.1 Centrifuge Tubes, plastic, 15-mL (plus 50-mL, ifnecessary).7.3.2 Polypropylene Bottles, 60 to 100 mL, with screw caps.7.3.3 Syringe Filters, 0.45-m or smaller pore size filters,for example, 13 or 25-mm diameter nylon filters, in plastichousings.7.3.4 Syringes
34、, plastic, 5-mL or 10-mL.7.3.5 Pipetters, mechanical, of assorted sizes as needed,with tolerances in accordance with EN ISO 8655-2.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.5The boldface numbers in parentheses refer
35、 to the list of references at the end ofthis standard.D7458 1427.3.6 Pipet Tips, plastic, disposable, of assorted sizes asneeded, with tolerances in accordance with EN ISO 8655-2.7.3.7 Fluorescence Cuvettes, disposable, low fluorescence,10-mm path length, transparent to UV/Visible radiation.7.3.8 La
36、bware, plastic (for example, beakers, flasks, gradu-ated cylinders, and so forth), of assorted sizes as needed.7.3.9 Forceps, plastic or plastic-coated.7.3.10 Personal Protective Wear, for example, respirators,masks, gloves, lab coats, safety eyewear, and so forth, asneeded.7.3.11 Thermometer, to at
37、 least 100C (accuracy 6 1C).7.3.12 Other general laboratory supplies as needed.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall beused. Unless otherwise indicated, it is intended that all reagentsconform to the specifications of the Committee on AnalyticalReagents of the American Chemi
38、cal Society where suchspecifications are available. Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall
39、be understood to mean reagent as defined byType I of Specification D1193 (ASTM Type I Water: minimumresistance of 18 M-cm or equivalent).8.3 Calibration Stock Solution1000 ppm beryllium indilute nitric acid.8.4 Ethylenediaminetetraacetic acid (EDTA) disodium saltdihydrate.8.5 L-lysine monohydrochlor
40、ide.8.6 10-hydroxybenzohquinoline-7-sulfonate (10-HBQS).8.7 Sodium hydroxide (NaOH).8.8 Extraction (or Dissolution) Solution3 % ammoniumbifluoride (NH4HF2) solution (aqueous) for dissolution ofberyllium in collected particulate matter. The solution may beprepared by dissolving 30 6 0.3 g of solid NH
41、4HF2in water toa total volume of 1000 mL. (WarningAmmonium bifluoridewill etch glass, so it is essential that all NH4HF2solutions becontained in plastic labware.)8.9 Detection Solution63.4 M 10-hydroxybenzohquinoline-7-sulfonate (10-HBQS) (5) / 2.5 mM ethylenedi-aminetetraacetic acid (EDTA)/50.8 mM
42、lysine monohydro-chloride (pH adjusted to 12.8 with NaOH): The aqueousdetection reagent is prepared by the addition of 12.5 mL of 2.5mM ethylenediaminetetraacetic acid (EDTA) disodium saltdihydrate and 25 mL of 107 mM L-lysine monohydrochlorideto 3 mL of 1.1 mM 10-hydroxybenzohquinoline-7-sulfonate(
43、10-HBQS). The pH is adjusted to 12.85 with addition ofsodium hydroxide and water added to a total of 50 mL.9. Hazards9.1 Ammonium bifluoride is highly corrosive, and is verytoxic when in contact with the skin. Effects to the skin,including irritation and burns, may not be felt for several hours.Avoi
44、d exposure by contact with the skin. Use suitable personalprotective equipment (including impermeable gloves and eyeprotection) when working with NH4HF2. See Appendix X1 forfurther pertinent safety information.10. Sample Collection and Transport10.1 Sample CollectionCollect samples in accordancewith
45、 applicable ASTM International standards for the type ofmedia (for example, soil, rock, sediment, fly ash) and thelocation being sampled (for example, surface, vadose zone).Refer to Guide D5730 in selecting applicable ASTM Interna-tional standards for sample collection.10.2 Sample TransportIf applic
46、able (that is, if samples aretransported to a different location prior to sample preparationand analysis), follow sampling chain-of-custody procedures todocument sample traceability. Make sure that the documenta-tion that accompanies the samples is suitable for a chain ofcustody to be established in
47、 accordance with Guide D4840.11. Procedure11.1 Specimen PreparationWear appropriate personalprotection during specimen preparation and analysis activities.Perform specimen preparation and analysis in a clean area thatis well removed from any possible beryllium contamination.11.1.1 Digestion of Sampl
48、es:11.1.1.1 Accurately weigh (to the nearest 0.1 mg) a 0.5-gram aliquot of sample into a polypropylene bottle. Close thelid and gently tap the lid to make sure that all of the aliquotfalls to the bottom of the bottle. The bottle size is typically 10to 50 mL larger than the liquid to be added.NOTE 2C
49、are should be taken to make sure that the aliquot(s) used arerepresentative of the soil, rock, sediment, or fly ash from which thesamples were taken. Guidance may be found in references (6-9).11.1.1.2 Remove the lid and, using a graduated cylinder,add 50 6 0.5 mL of 3 % ammonium bifluoride (NH4HF2)extraction solution (see 8.8). Replace the lid, making sure thelid is tight.11.1.1.3 Swirl the bottle to make sure that the specimen iscompletely wetted.11.1.1.4 Repeat steps 11.1.1.1 through 11.1.1.3 for all speci-mens.11.1.1.5 Place specimen bottles in a
