Federal Register - May 19, 2021
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Source: Federal Register
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Federal Register / Vol. 86, No. 95 / Wednesday, May 19, 2021 / Rules and Regulations
19 An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must be analyzed within 24 hours of collection, add the acid immediately see footnote 2. Soil and sediment samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and holding time requirements in the approved metals methods.
20 To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6. The allowance in this footnote supersedes preservation and holding time requirements in the approved hexavalent chromium methods, unless this supersession would compromise the measurement, in which case requirements in the method must be followed.
21 Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
22 Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later than 8 hours from time of collection.
23 For fecal coliform samples for sewage sludge biosolids only, the holding time is extended to 24 hours for the following sample types using either EPA Method 1680 LTBEC or 1681 A1: Class A composted, Class B aerobically digested, and Class B anaerobically digested.
24 The immediate filtration requirement in orthophosphate measurement is to assess the dissolved or bio-available form of orthophosphorus i.e., that which passes through a 0.45-micron filter, hence the requirement to filter the sample immediately upon collection i.e., within 15 minutes of collection.
3. Amend 136.6 by adding paragraph b4xxiii to read as follows:
136.6 Method modifications and analytical requirements.
b
4
xxiii When analyzing metals by inductively coupled plasma-atomic emission spectroscopy, inductively coupled plasma-mass spectrometry, and stabilized temperature graphite furnace atomic absorption, closed-vessel microwave digestion of wastewater samples is allowed as alternative
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Sample Preparation Procedure for Spectrochemical Determination of Total Recoverable Elements for the following elements: Aluminum, antimony, arsenic, barium, beryllium, boron, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, molybdenum, nickel, potassium, selenium, silver, sodium, thallium, tin, titanium, vanadium, zinc, provided the performance specifications in the relevant determinative method are met. Note that this list does not include Mercury. Each laboratory determining total recoverable metals is
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required to operate a formal quality control QC program. The minimum requirements include initial demonstration of capability, method detection limit MDL, analysis of reagent blanks, fortified blanks, matrix spike samples, and blind proficiency testing samples, as continuing quality control checks on performance. The laboratory is required to maintain performance records on file that define the quality of the data generated.
FR Doc. 202109596 Filed 51821; 8:45 am BILLING CODE 656050P
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