4.1 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 Method D1976, Practice D3919, Practice D4691, and Test Method D4190) or plasma-mass spectrometry (see Test Method D5673) and have been shown to give good recovery in the following matrices: industrial effluents; waste water treatment plant influents, sludges, dewatered sludges, and effluents; river and lake waters; and plant and animal tissues. Elements 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 sample's 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 D4309.1.1 Most atomic absorption and plasma emission spectroscopy, 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:  SectionsPractice A—Digestion with Mineral Acids and Elevated Pressure  8 through 13Practice B—Digestion with Mineral Acids and Heating at Atmospheric Pressure 14 through 19Practice C—In-Bottle Digestion with Mineral Acids 20 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 sample's 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 of a sample. It is the user's 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 in Guide D3856 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 mathematical conversion to inch-pound units that are provided for information only and are not considered standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 6.1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This practice is intended for the digestion of metals and metalloids in airborne dust and dust wipe samples collected during various activities performed in and around workplaces, buildings and related structures.5.2 This practice is applicable to the digestion of airborne dust and dust wipe samples collected in accordance with Test Method D4532, Guide D6062, Practice D7144 or Guide E1370 for airborne dust, and Practices D6966, D7296, D7822, or E1728 using wipes that may or may not conform to Specifications D7707 or E1792.5.2.1 This practice is applicable to the digestion of airborne dust sample filters that have been removed from their sampling cassettes which have been wiped to collect all dust adhering to the side walls and included in the hard-walled containers as part of the collected samples.5.2.2 This practice is applicable to the digestion of airborne dust samples that use acid-soluble cellulosic air sampling capsules with the entire contents of the cassettes transferred to hard-walled containers.5.2.3 This practice is applicable to the digestion of settled dust samples collected using wipe materials in hard-walled containers.5.3 Digestates prepared according to this practice are intended to be analyzed for metal and metalloid concentrations using spectrometric techniques such as inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), graphite furnace atomic absorption spectrometry (GFAAS), and flame atomic absorption spectrometry (FAAS) (see Test Methods D4185, D6785, D7035, D7439, E1613, E3193, and E3203), or for lead using electrochemical techniques such as anodic stripping voltammetry (see Practice E2051), or for beryllium using optical fluorescence detection (see Test Method D7202).5.4 Laboratories developing in-house test methods using this procedure shall determine precision and bias in accordance with the principles laid down by their accrediting agency.1.1 This practice covers the digestion of airborne and surface dust samples (collected using air and wipe sampling practices) and associated quality control (QC) samples for the determination of metals and metalloids by means of a mixture of dilute ammonium bifluoride and nitric acid.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This practice contains notes which are explanatory and not part of mandatory requirements of the standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Cyanide and hydrogen cyanide are highly toxic. Regulations have been established to require the monitoring of cyanide in industrial and domestic wastewaters and surface waters.45.2 This test method is applicable for natural water, saline waters, and wastewater effluent.5.3 This test method may be used for process control in wastewater treatment facilities.5.4 The spot test outlined in Test Methods D2036, Annex A1, can be used to detect cyanide and thiocyanate in water or wastewater, and to approximate its concentration.1.1 This test method is used for determining total cyanide in drinking and surface waters, as well as domestic and industrial wastes. Cyanide ion (CN–), hydrogen cyanide in water (HCN(aq)), and the cyano-complexes of zinc, copper, cadmium, mercury, nickel, silver, and iron may be determined by this test method. Cyanide ions from Au(I), Co(III), Pd(II), and Ru(II) complexes are only partially determined.1.2 The method detection limit (MDL) is 1.0 μg/L cyanide and the minimum level (ML) is 3 μg/L. The applicable range of the method is 3 to 500 μg/L cyanide using a 200-μL sample loop. Extend the range to analyze higher concentrations by sample dilution or changing the sample loop volume.1.3 This test method can be used by analysts experienced with equipment using segmented flow analysis (SFA) and flow injection analysis (FIA) or working under the close supervision of such qualified persons.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in 8.5 and Section 9.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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