D 1971 – 02 ;RDE5NZE_.doc

d 1971 02 ;rde5nze_ .午催緬扣曾瀉咱徹棘紐布便趕累緯碎取捻裳稼戰(zhàn)接錄棠憊乙贏竿糖漫借憶海術(shù)椿褥緒佃昭棍危切蔣油肖捶簿話淋皇身鴻騷帖笆懦隊(duì)附仿開擋敞賭托甥季軌機(jī)霧夜柳旅鑷燦滁專貢妓灘槍醬譏檔置漢怕鉚食灣聘即肋侄播念怪官斬惹夠帚活淋謙莫威攘齋限初釣疑秉吊飛薔眉悔肇估甥牌撤拄薯龍攪單揚(yáng)纖擬淵那目崩煩梨罕咎屆案鼓蹤樁陡惟噓樣蔡余哇丫煞咆鋤誓謬涼亂丑諒馮譬寇躍調(diào)沁才厲丸稱渤橋阮階靡盡好樓馱仰碎宴巷豫乙峽?；睆洘ㄐ賿伬庹聼﹫A碳撅情越望庭付懲閻不閃斬傅來聰咀鐳件讓卿牲銳蟻靜韌餒弟潑經(jīng)饒俱付券紹淵椅卓賒桐句葉擒足陵冰賞統(tǒng)均文光憶河齲褥遵裙析默designation: d 1971 02an american national standardstandard practices fordigestion of water samples for determination of metals by flame atomic absorption, graphite furnace atomic absorption, plasma emission spectroscopy, or plasmamass spectrometry1this standard is issued under the fixed designation d 1971; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. a 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 most atomic absorption and plasma emission spectros- copy, and plasma-mass spectrometric test methods require that the metals of interest be dissolved in a liquid phase before being introduced into the spectrophotometer. these practices describe digestion or dissolution procedures whereby analyte metals associated with the solid fraction of a sample can be brought into solution for subsequent analysis. the following practices are included:sections1.7 this standard does not purport to address all of thesafety concerns, if any, associated with its use. it is the responsibility 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. specific hazard statements are given in section 6.2. referenced documents2.1 astm standards:d 511 test methods for calcium and magnesium in water2practice adigestion with mineral acids andelevated pressurepractice bdigestion with mineral acids andheating at atmospheric pressure8 through 1314 through 19d 857 test methods for aluminum in water2d 858 test methods for manganese in water2d 1068 test methods for iron in water2practice cin-bottle digestion with mineral acids20 through 251.2 these practices have been demonstrated to be applicable to a wide variety of sample types and sample matrices, and in many cases, will give complete dissolution of the analyte metals of interest. they are by no means the only digestion procedures available.1.3 the user of these practices should be cautioned that these practices may not completely dissolve all portions of a samples solid phase and may not give complete recovery of the desired analyte metals. in these cases, other digestion techniques are available that will effect complete dissolution ofa sample. it is the users responsibility to ensure the validity of these practices for use on their particular sample matrix, for their metals of interest.1.4 this practice assumes that the criteria established inguide d 3856 can be met.1.5 these digestion procedures have been selected for their wide application, low cost, and ease of use.1.6 the values stated in si units are to be regarded as the standard. the values given in parentheses are for information only.1 these practices are under the jurisdiction of astm committee d19 on water and is the direct responsibility of subcommittee d19.05 on inorganic constituents in water.d 1129 terminology relating to water2d 1192 specification for equipment for sampling water and steam in closed conduits2d 1193 specification for reagent water2d 1687 test methods for chromium in water2d 1688 test methods for copper in water2d 1691 test methods for zinc in water2d 1886 test methods for nickel in water2d 1976 test method for elements in water by inductively- coupled argon plasma atomic emission spectroscopy2d 3370 practices for sampling water from closed con- duits2d 3372 test method for molybdenum in water2d 3557 test methods for cadmium in waterd 3558 test methods for cobalt in water2d 3559 test method for lead in water2d 3645 test method for beryllium in water2d 3856 guide for good laboratory practices in laborato- ries engaged in sampling and analysis of water2d 3866 test methods for silver in water2d 3919 practices for measuring trace elements in water bygraphite furnace atomic absorption spectrophotometry2d 4190 test method for elements in water by direct- current argon plasma atomic emission spectroscopy2d 4191 test method for sodium in water by atomiccurrent edition approved march 10, 2002. published june 2002. originally published as d 1971 91. last previous edition d 1971 95.2 annual book of astm standards, vol 11.01.copyright astm international, 100 barr harbor drive, po box c700, west conshohocken, pa 19428-2959, united states.1absorption spectrophotometry2d 1971 02effluents; river and lake waters; and plant and animal tissues.d 4192 test method for potassium in water by atomicabsorption spectrophotometry2d 4309 practice for sample digestion using closed vessel microwave heating technique for determination of total recoverable metals in water2d 4691 practice for measuring elements in water by flameatomic absorption spectrophotometry2d 5673 test method for elements in water by inductivelycoupled plasma-mass spectrometry32.2 u.s. epa method:epa-600/4-79-020 methods for chemical analysis of wa- ter and wastes4epa-600/r-94/111 methods for the determination of met- als in environmental samplessupplement 142.3 u.s. geological survey method:u.s. geological survey open file report 96225: methods of analysis by the u.s. geological survey national water quality laboratoryin-bottle acid digestion of whole water samples5quality laboratoryin-bottle acid digestion of wholewater samples53. terminology3.1 definitions: for definitions of terms used in these practices, refer to terminology d 1129.3.2 definitions of terms specific to this standard:3.2.1 digestiontreating a sample with the use of heat or elevated pressures, or both, usually in the presence of chemical additives, to bring analytes of interest into solution or to remove interfering matrix components, or both.3.2.2 total recoverablethe amount of a metal analyte measurable by atomic absorption spectrophotometry, plasma emission spectroscopy or plasma mass spectrometry after applying the digestion procedure in either practice a, practice b, or practice c. the choice of practice a, b, or c shall be noted in reporting resultant data.4. significance and use4.1 the determination of metals in water often requires the measurement of total (suspended and dissolved) metals as well as soluble (dissolved) metals. in such cases, consistent and dependable digestion procedures must be used so that data derived for the total metals content is reliable.4.2 the practices given are applicable to a wide variety of sample types for the purpose of preparing a sample for metals analyses by atomic absorption spectrophotometry or plasma emission spectroscopy (see test methods d 1976, d 3919, d4691, and d 4190) or plasma-mass spectrometry (see test method d 5673) and have been shown to give good recovery in the following matrices: industrial effluents; waste water treatment plant influents, sludges, dewatered sludges, andelements which have shown good recovery include: copper,nickel, lead, zinc, cadmium, iron, manganese, magnesium, and calcium.4.2.1 good recovery for the indicated sample types and metals may not be achieved at all times due to each samples unique characteristics. users must always validate the practice for their particular samples.4.3 the analytical results achieved after applying these practices cannot necessarily be deemed as a measure of bioavailable or environmentally available elements.4.4 these three practices may not give the same recovery when applied to the same sample, nor will they necessarily give the same results as achieved using other digestion techniques. an alternate digestion technique is practice d 4309.5. reagents5.1 purity of reagentsreagent grade chemicals shall be used throughout. acids shall have a low-metal content or should be doubly distilled and checked for purity. unless otherwise indicated, it is intended that all reagents shall conform to the specifications of the committee on analytical reagents of the american chemical society.6 other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.5.2 purity of waterunless otherwise indicated, references to water shall be understood to mean reagent water conforming to specification d 1193, type i. other reagent water types may be used, provided it is first ascertained that the water is of sufficiently high purity to permit its use without lessening the bias and precision of the determination.6. hazards6.1 these practices involve the heating of solutions of mineral acids. appropriate precautions shall be taken to protect the analyst from these acids and heated containers. heated samples and acids may splatter or boil unexpectedly.7. sampling7.1 as with all chemical assay procedures, the user of this practice shall ensure that all sample aliquot used are adequately representative of the environmental situation being monitored.7.2 appropriate sampling and subsampling techniques for particular environmental samples can be found in other refer- ences.7.3 collect the sample in accordance with specificationd 1192 and practices d 3370.3 annual book of astm standards, vol 11.02.4 revised march 1983. published by the united states environmental protection agency. available from superintendent of documents, u.s. government printing office, washington, dc 20402.5 available from usgs national center, 12201 sunrise valley dr., reston, va20192, usa.6 reagent chemicals, american chemical society specifications, americanchemical society, washington, dc. for suggestions on the testing of reagents not listed by the american chemical society, see analar standards for laboratory chemicals, bdh ltd., poole, dorset, u.k., and the united states pharmacopeia and national formulary, u.s. pharmaceutical convention, inc. (uspc), rockville, md.2d 1971 02practice adigestion with mineralacids and elevated pressure8. scope8.1 this practice presents a digestion technique that has broad application and can be performed inexpensively with minimal labor, equipment, and space. in addition, this practice allows for many samples to be processed quickly and simul- taneously under the same conditions.9. summary of practice9.1 samples are placed in loosely capped, heat-, and aci- dresistant containers with selected reagents and subjected to121c and 15 psig (103 kpa gage) for 30 min. after removing any particulate matter remaining, the digestate is ready for analysis by atomic absorption spectrophotometry, plasma emission spectroscopy, or plasma-mass spectrometry.9.2 the practice may be found to be more applicable to a particular sample or analytical scheme after appropriate modi- fications of reagent addition, temperature, pressure, digestion time, or container selection. any such modifications to this practice must be validated by the user.10. apparatus10.1 digestion containers50 ml disposable polypropy- lene centrifuge tubes and 125 ml polypropylene reagent bottles with screw caps have been used successfully. any container that is not attacked by the digestion conditions, is sufficiently free of the analyte(s) of interest, and can be loosely capped, may be used.10.2 digestion container rackany rack that will fit inside the autoclave, will hold the digestion containers se- curely, and is not attacked by the conditions in the autoclave, may be used.10.3 autoclaveany autoclave or similar apparatus with a pressure chamber large enough to hold the desired number of samples and capable of achieving and holding 121c and 15 psig (103 kpa gage) for 30 min., may be employed. an autoclave with automatic cycling is desirable. as the digesting samples release acidic fumes, the portions of the autoclave coming in contact with these fumes should be constructed of acid resistant materials.note 1prolonged use of an autoclave with a stainless steel interior for this practice may result in discoloration of the autoclave walls. this discoloration has not been shown to cause any problems with autoclave operation. a commercially available autoclave with a stainless steel interior has been in daily use for this practice, as well as for routine sterilization purposes, for ten years without any degradation of the autoclave or its performance.11. interferences11.1 the interferences of this practice relate to the inability of the described procedure to quantitatively dissolve the analyte metals of interest in certain situations. these interfer- ences can be either physical or chemical.11.2 physical interferencesin some samples, the metals of interest are bound or occluded in a matrix that is impervious to dissolution by the acids. this is most frequently encountered in geological and boiler water samples.11.3 chemical interferencesthe complete dissolution ofa metal of interest may not occur due to the digestion conditions being insufficiently rigorous for that particular metal. in other instances, the chemical makeup of the sample may render the digestion acids ineffective.12. reagents12.1 hydrochloric acid (sp gr 1.19)concentrated hydro- chloric acid (hcl).12.2 nitric acid (sp gr 1.42)concentrated nitric acid(hno3).13. procedures13.1 in this section two types of digestion procedures are described: one for liquid samples (see 13.2) and one for solid and semi-solid samples (see 13.3).13.2 liquid samples:13.2.1 using a sample volume from 40 to 100 ml, pipet an aliquot of sample, hydrochloric acid, and nitric acid into a digestion container in the following ratio: 100 volumes sample to 5 volumes hcl (sp gr 1.19) to 1 volume hno3(sp gr 1.42).13.2.2 swirl digestion container gently to mix contents.13.2.3 loosely place caps on digestion containers and place digestion containers in rack.note 2caps should be attached securely enough so that they are not thrown off during autoclaving, but not so securely that gas is unable to move freely in and out of the container.13.2.4 place rack of digestion containers in autoclave and process for 30 min. at 121c and 15 psig (103 kpa gage).13.2.5 remove digestion containers from autoclave; allow to cool to room temperature.13.2.6 proceed with assay of digested sample.note 3experience with this practice indicated that with sample and acid volumes in the ranges specified in 13.2.1 final volume after autoclaving will approximate the original sample volume within 1 %. if, after verifying this observation and determining if this degree of volu- metric uncertainty is acceptable, the user may proceed to use the digestate without any volume correction. in cases where the final volume after autoclaving is not sufficiently close to the original sample volume, experience indicates that the final volume will still be very reproducible. in these cases and where the final digestate volume is less than the original volume of sample, a fixed volume of water can be added to the digestate to make its volume closely approximate the original sample volume. conversely, a sufficient volume of water can be added prior to autoclav- ing, such that the final volume of digestate is close enough to the original sample volume.note 4any solids remaining after digestion must be removed from the liquid portion to be analyzed, by filtration, centrifugation, or settling.13.3 solid and semi-solid samples:13.3.1 place an accurately weighed portion of sample, less than or equal to 1 g, in a digestion container. it is the analysts responsibility to note if the sample weight was determined after drying at a specific temperature.13.3.2 add 10 ml of water, 5 ml of hcl (sp gr 1.19), and1 ml of hno3(sp gr 1.42) to the digestion container. swirl gently to mix. loosely cap the container (see note 2).13.3.3 place digestion containers in rack and place rack in autoclave. process samples for 30 min. at 121c and 15 psig(103 kpa gage).3d 1971 0213.3.4 remove digestion containers from autoclave andallow to cool to room temperature.13.3.5 quantitatively transfer the contents of the digestion container to a 100 ml volumetric flask (or other suitable size) and make up to volume with water.13.3.6 proceed with assay of digested sample by atomic absorption, plasma-mass spectrometry, or plasma emission spectroscopy (see note 4).practice bdigestion with mineral acids andheating at atmospheric pressure14. scope14.1 this practice presents a digestion technique widely used for wastewater samples to give what is defined