EN 13656:2020

SLOVENSKI STANDARD
01-december-2020
Nadomešča:
SIST EN 13656:2004
Tla, obdelani biološki odpadki, blato in odpadki - Razklop z zmesjo klorovodikove
kisline (HCl), dušikove(V) kisline (HNO3) in tetrafluoroborove kisline (HBF4) ali
fluorovodikove kisline (HF) za določevanje elementov
Soil, treated biowaste, sludge and waste - Digestion with a hydrochloric (HCl), nitric
(HNO3) and tetrafluoroboric (HBF4) or hydrofluoric (HF) acid mixture for subsequent
determination of elements
Boden, behandelter Bioabfall, Schlamm und Abfall - Aufschluss mit einem Gemisch aus
Salzsäure (HCl), Salpetersäure (HNO3) und Tetrafluorborsäure (HBF4) oder
Fluorwasserstoffsäure (HF) für die anschließende Bestimmung der Elemente
Sols, bio-déchets traités, boues et déchets - Digestion par un mélange d’acides
chlorhydrique (HCl), nitrique (HNO3) et tétrafluoroborique (HBF4) ou fluorhydrique (HF)
pour la détermination ultérieure des éléments
Ta slovenski standard je istoveten z: EN 13656:2020
ICS:
13.030.40 Naprave in oprema za Installations and equipment
odstranjevanje in obdelavo for waste disposal and
odpadkov treatment
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 13656
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2020
EUROPÄISCHE NORM
ICS 13.030.40 Supersedes EN 13656:2002
English Version
Soil, treated biowaste, sludge and waste - Digestion with a
hydrochloric (HCl), nitric (HNO ) and tetrafluoroboric
(HBF ) or hydrofluoric (HF) acid mixture for subsequent
determination of elements
Sols, bio-déchets traités, boues et déchets - Digestion Boden, behandelter Bioabfall, Schlamm und Abfall -
par un mélange d'acides chlorhydrique (HCl), nitrique Aufschluss mit einem Gemisch aus Salzsäure (HCl),
(HNO ) et tétrafluoroborique (HBF ) ou fluorhydrique Salpetersäure (HNO ) und Tetrafluorborsäure (HBF )
3 4 3 4
(HF) pour la détermination ultérieure des éléments oder Fluorwasserstoffsäure (HF) für die anschließende
Bestimmung der Elemente
This European Standard was approved by CEN on 21 September 2020.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATIO N

EUROPÄISCHES KOMITEE FÜR NORMUN G

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 13656:2020 E
worldwide for CEN national Members.

Content Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 6
5 Interferences and sources of errors . 7
5.1 General information . 7
5.2 Closed vessel system for microwave digestion . 7
6 Reagents . 7
7 Apparatus . 8
8 Procedure . 9
8.1 General . 9
8.2 Blank test . 9
8.3 Method A: Heating block digestion using HCl, HNO and HBF . 9
3 4
8.4 Method B: Microwave digestion . 10
9 Test report . 12
Annex A (normative) Calibration of the power adjustment . 13
Annex B (informative) Repeatability and reproducibility data – Method A and B1 . 14
Annex C (informative) Repeatability and reproducibility data – Method B2 . 23
Bibliography. 36

European foreword
This document (EN 13656:2020) has been prepared by Technical Committee CEN/TC 444 “Environmental
characterization of solid matrices”, of which the secretariat is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by May 2021 and conflicting national standards shall be withdrawn at
the latest by May 2021.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 13656:2002.
In comparison with EN 13656:2002, the following modifications have been made:
— addition of HBF4 as acid. For safety reasons the use of HBF4 is preferred over HF;
— addition of a heating block digestion procedure;
— addition of a microwave digestion procedure temperature-controlled;
— removal of the microwave digestion with semi-open vessel system.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United
Kingdom.
Introduction
The methods specified in this document are providing a multi-element digestion of soil, treated biowaste,
sludge and waste prior to analysis. Elements extractable by this procedure can in many instances be
described as “total”, although this will be sample dependent. On the other hand, they cannot be regarded
as available for leaching, as the extraction procedure is too vigorous to represent natural processes.
This document is validated for several types of matrices as indicated in Table 1.
Table 1 — Matrices for which EN 13656 is validated
Materials used in the validation test Validated for digestion Validated for digestion
with HCl:HNO :HBF with HCl:HNO :HF
3 4 3
(see Annex B) (see Annex C)
City waste incineration ash X X
(BCR176/BCR176R)
Ink waste sludge (organic matrix) X X
Electronic industry sludge (“metallic” X X
matrix)
Sediment X
Coal fly ash X
Steel slag X
Copper slag X
City waste incineration fly ash  X
(“oxidised” matrix)
City waste incineration bottom ash  X
(“silicate” matrix)
Sewage sludge (BCR 146R)  X
WARNING — Persons using this document should be familiar with usual laboratory practice. Most
of the reagents used in this document are extremely corrosive and very toxic. Safety precautions
are absolutely necessary, not only due to the strong corrosive reagents employed, but also to the
high temperature and pressures employed.
The use of laboratory-grade microwave equipment with isolated and corrosion resistant safety
devices is essential. Domestic (kitchen) type microwave ovens should not be used, as corrosion by
acid vapours may compromise the function of the safety devices and prevent the microwave
magnetron from shutting off when the door is open, which could result in operator significant
hazardous exposure to microwave energy.
All procedures should be performed in a fume hood or in closed force-ventilated equipment. By the
use of strong oxidising reagents, the formation of explosive organic intermediates is possible,
especially when dealing with samples with a high organic content. Do not open pressurized vessels
before they have cooled down. Avoid contact with the chemicals and the gaseous reaction products.
IMPORTANT — It is absolutely essential that tests conducted according to this document be carried
out by suitably trained staff. People performing the test should be informed on the specific risks
associated with the use of HBF and HF.
1 Scope
This document specifies three methods for the digestion of soil, treated biowaste, sludge and waste by the
use of an acid mixture composed of hydrochloric (HCl), nitric (HNO ) and tetrafluoroboric (HBF ) or
3 4
hydrochloric (HCl), nitric (HNO ) and hydrofluoric (HF) acid as the digestion solution.
Digestion with these acids is effectively considered as a total decomposition of the sample. Elements
extractable by this procedure can in many instances be described as “total”, although this will be sample
dependent.
This document is applicable for the following elements:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), cadmium (Cd), calcium (Ca),
chromium (Cr), cobalt (Co), copper (Cu), iron (Fe), lead (Pb), magnesium (Mg), manganese (Mn), mercury
(Hg), molybdenum (Mo), nickel (Ni), phosphorus (P), potassium (K), selenium (Se), silver (Ag), sodium
(Na), strontium (Sr), sulfur (S), tellurium (Te), thallium (Tl), tin (Sn), titanium (Ti), vanadium (V), and
zinc (Zn).
This document can also be applied for the digestion of other elements, provided the user has verified the
applicability.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
EN 15002, Characterization of waste - Preparation of test portions from the laboratory sample
EN 15934, Sludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination of
dry residue or water content
EN 16179, Sludge, treated biowaste and soil - Guidance for sample pretreatment
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
3.1
digestion
mineralization of the organic matter of a sample and dissolution of its mineral part, more or less completely,
when reacting with a reagent mixture
3.2
dry residue
remaining mass fraction of a sample after a drying process at 105 °C under specified conditions
[SOURCE: EN 15934:2012, 3.1]
3.3
dry matter fraction
(dm)
mass fraction of a sample excluding water expressed as mass fraction calculated by determination of dry
residue or water content
[SOURCE: EN 15934:2012, 3.3]
3.4
laboratory sample
sample intended for laboratory inspection of testing
[SOURCE: EN ISO 11074:2015, 4.3.7]
3.5
sample
portion of material selected from a larger quantity of material
3.6
test portion
quantity of material, of proper size for measurement of the concentration or other property of interest,
removed from the test sample
Note 1 to entry: The test portion may be taken from the laboratory sample directly if no preparation of sample is
required (e.g. with liquids), but usually it is taken from the prepared test sample.
Note 2 to entry: A unit or increment of proper homogeneity, size and fineness, needing no further preparation, may
be a test portion.
[SOURCE: EN ISO 11074:2015, 4.3.15]
3.7
test sample
portion of material resulting from the labo
...