美国环保署 EPA-Method 3051A 微波辅助酸消化沉积物、污泥、土壤和油 2007

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3051A - 1 Revision 1

February 2007

METHOD 3051A

MICROWAVE ASSISTED ACID DIGESTION OF

SEDIMENTS, SLUDGES, SOILS, AND OILS

SW-846 is not intended to be an analytical training manual. Therefore, method

procedures are written based on the assumption that they will be performed by analysts who are

formally trained in at least the basic principles of chemical analysis and in the use of the subject

technology.

In addition, SW-846 methods, with the exception of required method use for the analysis

of method-defined parameters, are intended to be guidance methods which contain general

information on how to perform an analytical procedure or technique which a laboratory can use

as a basic starting point for generating its own detailed Standard Operating Procedure (SOP),

either for its own general use or for a specific project application. The performance data

included in this method are for guidance purposes only, and are not intended to be and must

not be used as absolute QC acceptance criteria for purposes of laboratory accreditation.

1.0 SCOPE AND APPLICATION

1.1 This microwave extraction method is designed to mimic extraction using

conventional heating with nitric acid (HNO3), or alternatively, nitric acid and hydrochloric acid

(HCl), according to EPA Method 200.2 and Method 3050. Since this method is not intended to

accomplish total decomposition of the sample, the extracted analyte concentrations may not

reflect the total content in the sample. This method is applicable to the microwave-assisted acid

extraction/dissolution‡ of sediments, sludges, soils, and oils for the following elements:

Element CAS Registry No. a

*Aluminum (Al) 7429-90-5

*Antimony (Sb) 7440-36-0

Arsenic (As) 7440-38-2

*Barium (Ba) 7440-39-3

*Beryllium (Be) 7440-41-7

Boron (B) 7440-42-8

Cadmium (Cd) 7440-43-9

Calcium (Ca) 7440-70-2

*Chromium (Cr) 7440-47-3

Cobalt (Co) 7440-48-4

Copper (Cu) 7440-50-8

*Iron (Fe) 7439-89-6

Element CAS Registry No. a

3051A - 2 Revision 1

February 2007

Lead (Pb) 7439-92-1

*Magnesium (Mg) 7439-95-4

Manganese (Mn) 7439-96-5

Mercury (Hg) 7439-97-6

Molybdenum (Mo) 7439-98-7

Nickel (Ni) 7440-02-0

Potassium (K) 7440-09-7

Selenium (Se) 7782-49-2

*Silver (Ag) 7440-22-4

Sodium (Na) 7440-23-5

Strontium (Sr) 7440-24-6

Thallium (Tl) 7440-28-0

*Vanadium (V) 7440-62-2

Zinc (Zn) 7440-66-6

a Chemical Abstract Service Registry Number

*Indicates elements which typically require the addition of HCl to achieve

equivalent results with Method 3050, as noted in Ref. 3.

‡Note: For matrices such as certain types of oils, this method may or may not

provide total sample dissolution. For other matrices, such as soils and sediments,

it should be considered an extraction method. Other elements and matrices may

be analyzed by this method if performance is demonstrated for the analyte of

interest, in the matrices of interest, at the concentration levels of interest (see

Sec. 9.0).

1.2 This method is provided as an alternative to EPA Method 200.2 and Method 3050.

This method provides options for improving the performance for certain analytes, such as

antimony, iron, aluminum, and silver by the addition of hydrochloric acid, when necessary. It is

intended to provide a rapid multi-element acid extraction or dissolution prior to analysis so that

decisions can be made about materials and site cleanup levels, the need for TCLP testing of a

waste (see Method 1311), and whether a BDAT process is providing acceptable performance.

Digests produced by the method are suitable for analysis by flame atomic absorption

spectrophotometry (FLAA), graphite furnace atomic absorption spectrophotometry (GFAA),

inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled

plasma mass spectrometry (ICP-MS). However, the addition of HCl may limit the quantitation

methods, or increase the difficulties of quantitation with some techniques.

Due to the rapid advances in microwave technology, consult your manufacturer's

recommended instructions for guidance on their microwave digestion system.

3051A - 3 Revision 1

February 2007

1.3 Prior to employing this method, analysts are advised to consult the determinative

method that may be employed in the overall analysis for additional information on quality control

procedures, development of QC acceptance criteria, calculations, and general guidance.

Analysts also should consult the disclaimer statement at the front of the manual and the

information in Chapter Two for guidance on the intended flexibility in the choice of methods,

apparatus, materials, reagents, and supplies, and on the responsibilities of the analyst for

demonstrating that the techniques employed are appropriate for the analytes of interest, in the

matrix of interest, and at the levels of concern.

In addition, analysts and data users are advised that, except where explicitly specified in a

regulation, the use of SW-846 methods is not mandatory in response to Federal testing

requirements. The information contained in this method is provided by EPA as guidance to be

used by the analyst and the regulated community in making judgments necessary to generate

results that meet the data quality objectives for the intended application.

1.4 Use of this method is restricted to use by, or under supervision of, properly

personnel experienced and trained in the use of microwave digestion systems. Each analyst

must demonstrate the ability to generate acceptable results with this method.

2.0 SUMMARY OF METHOD

A representative sample is extracted and/or dissolved in concentrated nitric acid, or

alternatively, concentrated nitric acid and concentrated hydrochloric acid using microwave

heating with a suitable laboratory microwave unit. The sample and acid(s) are placed in a

fluorocarbon polymer (PFA or TFM) or quartz microwave vessel or vessel liner. The vessel is

sealed and heated in the microwave unit for a specified period of time. After cooling, the vessel

contents are filtered, centrifuged, or allowed to settle and then diluted to volume and analyzed

by the appropriate determinative method.

3.0 DEFINITIONS

Refer to Chapter One, Chapter Three and the manufacturer's instructions for definitions

that may be relevant to this procedure.

4.0 INTERFERENCES

4.1 Solvents, reagents, glassware, and other sample processing hardware may yield

artifacts and/or interferences to sample analysis. All of these materials must be demonstrated

to be free from interferences under the conditions of the analysis by analyzing method blanks.

Specific selection of reagents and purification of solvents by distillation in all-glass systems may

be necessary. Refer to each method to be used for specific guidance on quality control

procedures and to Chapter Three for general guidance on the cleaning of glassware. Also refer

to the determinative methods to be used for a discussion of interferences.

4.2 Very reactive samples or volatile materials may create high pressures due to the

evolution of gaseous digestion products. This may cause venting of the vessels with potential

loss of sample and/or analytes. The complete decomposition of either carbonates, or carbon

based samples, may produce enough pressure to vent the vessel if the sample size is greater

than 0.25 g (depending on the pressure capability of the vessel). Variations of the method to

accommodate very reactive materials are specifically addressed in Sec. 11.3.3.

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摘要：

美国环保署 EPA Method 3051A（2007）规定了利用微波辅助酸消化处理沉积物、污泥、土壤和油类等环境样品的标准方法，是痕量金属与元素分析前处理的重要依据。该方法通过密闭微波加热与酸体系反应，快速、高效地破坏有机质和矿物基体，使目标金属元素转入溶液，便于后续采用ICP-OES、ICP-MS或AAS进行测定。其适用领域涵盖环境监测、污染场地调查、土壤修复评估、固废与油类检测及实验室质量控制。采用 EPA 3051A 有助于提升沉积物、污泥、土壤和油样前处理效率、降低交叉污染风险，并满足

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美国环保署 EPA-Method 3051A 微波辅助酸消化沉积物、污泥、土壤和油 2007

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