HORIZONTAL factsheet
PAH
version: 2/12/2016
SUBJECT
Determination of PAH
HORIZONTAL number
11
Matrices
Work package
Soil, sludge, biowaste, compost, waste
.ISO13877, ISOFDIS18727, DIN 384114 S 23,
US EPA 8100, 8310, 8270 B, ISO 17993
.........................................
CEN TC 345, CEN TC 308, CEN TC 223, ISO TC
190, CEN TC 292
5 Organic parameters
Project
STREP FP6 HORIZONTAL-ORG
Expert
Dr Tin Win
Organisation
BAM
Country
Germany
Email
Status
tin.win@bam.de
Existing standards used as basis
Standardisation Committees
Desk study First
Comments Phase I
Final version
Phase II Ruggedness
30 August 2003
October 2003
31 January 2004
Ongoing work
www.ecn.nl/horizontal
Completion due 31-03-05
Second consultation
Completion due 30-06-05
Validation
Completion due 31-03-06
Transfer to BT/TF151
Foreseen 30-06-06
Summary of PAH procedure
HORIZONTAL factsheet
PAH
version: 2/12/2016
Max 1/2 page
A horizontal method applicable for all environmental solid matrices of different PAHcontamination levels ( soil, waste, sludge and bio waste) with modules for extraction and
clean up followed by two alternative detection techniques HPLC-UV/FLD and GC/MS.
16 selected PAH according to EPA 610 are to be determined. 3 extraction methods are
described. Soxhlet extraction (Pressurised liquid extraction) with toluene for high
contaminated soil and waste sample. Shaking with acetone/hexane for soil, bio waste ,sludge
sediment and compost. Shaking with acetone/hexane/NaCl for wet samples( water content
less than 50 %) of soil like materials (peat), bio waste and compost with high organic
matter. Clean up is only necessary to remove the present disturbing components. When they
are not present, clean-up is not necessary .Clean up steps with GPC, DMSO/cyclohexane
liquid/liquid partition , and with desactivated Silica gel or aluminium oxide are described.
For the determination of selected PAH by GC-MS the internal standard method using
internal standards (deuterated or 13C PAH ) and by HPLC-UV/FLD the external standard
method is given. Performance criteria for extraction and clean up by recovery checks of
internal standards as well as examples of experimental conditions for GC and HPLC column
for satisfactory separation of critical pairs pf PAH are described.
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Placement of PAH method in overall structure HORIZONTAL
HORIZONTAL factsheet
PAH
version: 2/12/2016
SLUDGE, SOIL, TREATED BIOWASTE AND RELATED
WASTES
SAMPLING
IN-SITU ,TRANSPORT, STORAGE
SAMPLE PRETREATMENT - INORG
INORGANIC
CONSTITUENTS
PHYSICAL
PROPERTIES
SAMPLE PRETREATMENT - ORG & BIOL
LEACHING
ORGANIC
PARAMETERS
SAMPLE PRETREATMENT
- HYG
BIOLOGICAL
PARAMETERS
HYGIENIC
PARAMETERS
PAH
pH
Characterisation
leaching tests
Bulkdensity
Impurities(e.g
glass, plastic)
E. Coli
Stability(bio)
Salmonella
Germinating
w eed seeds
Clostridium
Phytotoxicity
Enterococci
AOX
Electrical
conductivity
Compliance
leaching tests
Drymatter
PCB
Organicmatter*
Solidity
LAS, NP,NPE
Nutrients N, P,
K*
Thixotropic
behaviour
Trace elements
solid *
Piling
behaviour
Trace elements
determination*
Flow ability
DEPH, DBP
Helminth ova
BFR
Rapid methods
PCCD/PCDF
Soluble P
Virussesand
bacteriophages
Pharmaceuticals
Plant
Pathogens
Position of PAH method in the sequence of steps from sampling to reporting
Sampling Taking of
plan
sample
Sampling
strategy
Transport & Preparation
storage
of test
portion
Sampling of 1)
sludge and
biowaste
2)
Extraction/
Leaching
Pre-treatment
Extraction of Pre-treatment
organic
organics 5)
parameters 5)
Detection &
Summary
Quantification, reports
Enumeration
Measurement
of PAH
Summary of
organic
parameter
composition 3)
Sampling of
soil in the
field 4)
1)Sample conservation, storage and transport are issues that generally are covered in as the final step in sampling standards
2) Preparation of the test portion from a laboratory sample is sometimes part of the next step (digestion or analysis preparation) or can
be covered in a separate standard
3) Summary of test results is a concise summary of the relevant data for the end-user, which can be merged in an overall test report
covering all aspects relevant for the given situation.
4) After defining sampling strategy based on the question to be answered either one of the sampling standards will generally apply. All
the following steps will be the same for either route.
5) It is at present not clear where extraction of organic parameters begins and pre-treatment ends. It seems that pre-treatment now includes
the extraction step.
Major issues of discussion
Equivalence of two detection methods HPLC-UV/FLD and GC/MS as well as extraction
capability of different extraction methods for the determination of PAH . Ruggedness test for
suitability and limits of application of the stated methods for all kind of relevant matrices.
Reducing of validation work load for all combination of methods and matrices. Availability
and gap analysis of existing validation data and identification of needs of materials for
specific matrices for setting priorities for the coming validation interlaboratory comparison.
HORIZONTAL factsheet
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PAH
version: 2/12/2016