HORIZONTAL Factsheet
BFR
version: 2/13/2016
SUBJECT
Determination of BFR
HORIZONTAL number
27
Matrices
Soil, sludge, waste, …..
Existing standards used as basis
..........................................
CEN/TC 292, CEN/TC 308, CEN/TC 345, ISO/TC
190, ……
5 Organic parameters
Standardisation Committees
Work package
STREP FP6 HORIZONTAL-ORG
Dr. Damià Barceló, Dr Ethel Eljarrat and Dr Goran
Marsh
Project
Expert
Organisation
CSIC
Country
Spain
Email
Status
dbcqam@cid.csic.es
Desk study First
Comments Phase I
Final version
Phase II Ruggedness
October 2004
January 2005
……..
www.ecn.nl/horizontal
Completion due 31-03-05
Second consultation
Completion due 30-06-05
Validation
Completion due 30-04-06
Transfer to BT/TF151
Foreseen 31-07-06
Summary of BFR procedure
The solid matrices are freeze dried. Lyophilized samples are ground and homogenized by
sieving through a stainless steel 0.2-mm sieve, and stored in sealed containers at -20ºC until
analysis. One gram dry weight of samples, are spiked with PCB-209. Extraction is preformed
on a pressurized liquid extraction (PLE) instrument. A 22 mL extraction cell is loaded by
inserting two cellulose filters into the cell outlet, followed by 6 g of alumina. Spiked samples
were ground with alumina and cooper (1:2:2). Mixtures were loaded into the extraction cell
on top of alumina. The dead volume was filled with Hydromatrix. The mixtures are extracted
(2 × 10 min) with hexane:CH2Cl2, 1:1 (tot. ca. 35 mL) at a temperature of 100ºC and a
pressure at 1500 psi. Extracts were finally concentrated to incipient dryness and re-dissolved
with 250 µL of CH2Cl2 prior to the analysis by GC-NCI-MS.
GC-NCI-MS analysis of mono- to heptaBDEs is performed on a non-polar “DB-5 type” of
GC capillary column, containing 5% phenyl methyl (30 m × 0.25 mm i.d., 0.25 µm film
thickness). Injections are made in the splitless mode with a ion source temperature at 250ºC.
Ammonia is used as the chemical ionization moderating gas at an ion source pressure of 1.9
10-4 torr. For the determination of BDE-209, a non-polar “DB-5 type” of GC capillary
column, 15 m × 0.25 mm i.d., 0.25 µm film thickness, containing 5% phenyl methyl siloxane
capillary column is used with helium as the carrier gas at 10 psi. Both experiments are carried
out monitoring the two most abundant isotope peaks from the mass spectra corresponding to
m/z = 79 and 81 ([Br]-). Confirmation criteria for the detection and quantification of PBDEs
include the following: (a) all m/z monitored for a given analyte should maximize
simultaneously  1s, with signal to noise ratio  3 for each; (b) the ratio between the two
monitored ions should be within 15% of the theoretical. Quantification of mono- to hepta-
HORIZONTAL Factsheet
BFR
version: 2/13/2016
BDEs is carried out by internal standard procedure with the PCB-209 as internal standard,
whereas BDE-209 was quantified using the external standard method. Recoveries from 47 to
82% were obtained for spiked tri- to heptaBDEs with relative standard deviations ranging
from 1-14%. Detection limits for tri- to heptaBDEs were between 1 and 46 pg/g dry weight
and between 30-110 pg/g dry weight for BDE-209.
Placement of BFR method in overall structure HORIZONTAL
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
BIOLOGICAL
PARAMETERS
SAMPLE PRETREATMENT
- HYG
HYGIENIC
PARAMETERS
PAH
pH
Bulk density
Characterisation
leaching tests
Impurities (e.g
glass, plastic)
E. Coli
Stability (bio)
Salmonella
Germinating
weed seeds
Clostridium
Phytotoxicity
Enterococci
AOX
Electrical
conductivity
Dry matter
Compliance
leaching tests
PCB
Organic matter*
Solidity
LAS, NP,NPE
Nutrients N, P,
K*
Thixotropic
behaviour
DEPH, DBP
Trace elements
solid *
Trace elements
determination*
Piling
behaviour
Helminth ova
BFR
Flowability
Rapid methods
PCCD/PCDF
Soluble P
Pharmaceuticals
Virusses and
bacteriophages
Plant
Pathogens
Position of BFR method in the sequence of steps from sampling to reporting
Sampling Taking of
plan
sample
Transport & Preparation
storage
of test
portion
Extraction/
Leaching
Pre-treatment
Detection &
Summary
Quantification, reports
Enumeration
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.
HORIZONTAL Factsheet
BFR
version: 2/13/2016
Major issues of discussion
 Regarding extraction, at this stage we do not know if we are going to choose Soxhlet
or PLE or both in the standard.

The described BFR procedure is working on PBDE analysis of sediment and soil
samples. However, the procedure needs to be validated for sewage sludge and biowaste samples.