CORRIGENDUM

to the certification reports on BCR-032

EUR 6807 EN and EUR 8537 EN

As a result of the revision of the certificates in May 2007, certified values and uncertainties should
read as follows:

NATURAL MOROCCAN PHOSPHATE ROCK

(Phosphorite)
Mass fraction based on dry mass Number of
1) 2) accepted
Certified value Uncertainty individual
[g/kg] [g/kg] measurements
Ca expressed as CaO 518 4 70
Total P expressed as P2O5 329.8 1.7 85
Carbonate Carbon expressed as CO2 51.0 0.8 60
F 40.4 0.6 80
Si expressed as SiO2 20.9 1.2 60
Total S expressed as SO3 18.4 0.8 75
Al expressed as Al2O3 5.5 0.6 80
Mg expressed as MgO 4.0 0.1 65
Fe expressed as Fe2O3 2.3 0.1 65
1)
The certified value is the unweighted mean of individual measurements obtained by different laboratories. The
certified value is traceable to SI.
2)
The uncertainty is estimated standard deviation of reproducibility which. It accounts for the precision and bias of
the participating laboratories as well as for any inhomogeneity of the material.
 Indicative Values
Mass fraction based on dry mass Number of
Certified value 1)
Uncertainty 2) accepted sets
[mg/kg] [mg/kg] of data p

As 9.5 0.5 7
B 22.6 2.2 6
Cd 20.8 0.7 12
Cr 257 16 12
Co 0.59 0.06 9
Cu 33.7 1.4 14
Hg 0.055 0.011 6
Mn 18.8 1.3 13
Ni 34.6 1.9 11
Ti 171 10 10
V 153 7 12
Zn 253 6 9
1) This value is the unweighted mean of p accepted sets of results. The certified value is traceable to SI.
2) The 95% confidence interval is a measure of the uncertainty and is applicable when the reference material is
used for calibration purposes.
When the reference material is used to assess the performance of a method, the user should refer to the
recommendations laid down in the last chapter (instructions for use) of the certification report. In particular he should
use the values of the within-laboratory set standard deviation (SW), and of the between-laboratory set standard
deviation (SB) given there.

Consequently certified values and uncertainties should read accordingly.

May 2007
Additional Material Information for BCR–032

In 2004, the Laboratory of the Rural, Water and Ecosystem Resources Unit at the JRC's
Institute for Environment and Sustainability (IES) performed a series of measurements on the
following CRMs: BCR-032, BCR-033, BCR-060, BCR-062, BCR-113, BCR-114, BCR-129,
BCR-142R, BCR-143R, BCR-144R, BCR-145R, BCR-146R, BCR-178, BCR-179, BCR-277R,
ERM-CE278, BCR-279, BCR-280R, BCR-320R, BCR-402, BCR-414, BCR-482, BCR-597,
ERM-CC690. The goal of these measurements was to provide CRM users with more
information on the matrix composition of these materials (SWCT-Report N° 02/10/2004), useful
to understand possible effects on the determination of the certified values. In most cases, the
respective analyses were carried out under conditions of intermediate precision, i.e. spread over
different units and over different days of analysis. This information can be used to complement
the information of the respective certificates of these materials.
All data are to be taken as informative values only.

Methods
X-ray fluorescence spectrometry
XRF-measurements were performed using a sequential wavelength-dispersive
XRF-Spectrometer AXS SRS 3400 WDXRF (Bruker), equipped with a Rh-Tube. Calibration,
analysis and quantification were carried out using the software SpectraPlus V 1.5.3. Signals
were automatically corrected for interferences using the aforementioned software. The
multivariate calibration curves were developed using certified values of analogue CRMs.
CHN
All measurements were done using a CE NCS 2500 Elemental Analyzer (FISONS® Instruments).
Calibration was done using 2,5-Bis(5-tert-butyl-benzoxazol-2-yl)thiophene (C%:72.53; H%: 6.09;
N%: 6.51; O%: 7.43; S%: 7.44.) as calibration standard.
Total carbon content
Total carbon content and Organic carbon content was measured using an Automatic Carbon and
Sulphur Determinator CS 900 (ELTRA). Aliquots were weighed directly into ceramic crucibles.
Combustion was achieved in a stream of oxygen. Detection was done using an IR-cell. The device
was calibrated using pure calcium carbonate, purity > 99.5 % (Fluka, Switzerland).
Organic carbon content
Total carbon content and Organic carbon content was measured using an Automatic Carbon and
Sulphur Determinator CS 900 (ELTRA). Aliquots were weighed directly into ceramic crucibles.
Combustion was achieved in a stream of oxygen. Detection was done using infrared spectrometry.
For the determination of the organic carbon content the solid samples were acidified with 1 % HCl
solution in order to destroy inorganic carbon prior to the measurements.
Mercury
Hg was measured by cold vapor atomic absorption spectrometry (CVAAS) using an AMA 245
device (ELTRA). Calibration was obtained using a Carlo Erba Hg-Standard for AAS (N° 497551)
in 2.5 % HCl: for calibration.
Results
The mean values of the observed concentrations are shown below. It should be highlighted
that these results are not certified values and are informative only.

BCR-032

Analyte Unit Average Standard deviation Replicates

Si (1) g / 100 g < 0.02 4

(1)
Al g / 100 g < 0.03 4
Ca (1) g / 100 g 27.71 0.09 4
K (1) g / 100 g < 0.04 4
(1)
Fe g / 100 g < 0.04 4
(1)
Mg g / 100 g 0.24 0.00 4
(1)
Ti mg / kg < 12 4
P (1) mg / kg 107 590 170 4
Pb (1) mg / kg 5.8 1.3 4
(1)
Zn mg / kg 164.0 1.9 4
(1)
Cu mg / kg <2 4
Ni (1) mg / kg 39.5 2.0 4
Mn (1) mg / kg 2 2
Cr (1) mg / kg 119.5 1.0 4
(1)
Na g / 100 g 0.52 0.00 4
(2)
N g / 100 g 0.018 7 0.001 5 12
C (2) g / 100 g 1.488 0.028 12
Corg (3) g / 100 g 0.98 0.06 6
(3)
Ctot g / 100 g 1.526 0.010 6

(1) determined by WDXR;

(2) determined using CHN-analyser;
(3) determined using carbon/sulphur analyser.
Additional Material Information for BCR–032

In 2004, the Laboratory of the Rural, Water and Ecosystem Resources Unit at the JRC's
Institute for Environment and Sustainability (IES) performed a series of measurements on the
following CRMs: BCR-032, BCR-033, BCR-060, BCR-062, BCR-113, BCR-114, BCR-129,
BCR-142R, BCR-143R, BCR-144R, BCR-145R, BCR-146R, BCR-178, BCR-179, BCR-277R,
ERM-CE278, BCR-279, BCR-280R, BCR-320R, BCR-402, BCR-414, BCR-482, BCR-597,
ERM-CC690. The goal of these measurements was to provide CRM users with more
information on the matrix composition of these materials (SWCT-Report N° 02/10/2004), useful
to understand possible effects on the determination of the certified values. In most cases, the
respective analyses were carried out under conditions of intermediate precision, i.e. spread over
different units and over different days of analysis. This information can be used to complement
the information of the respective certificates of these materials.
All data are to be taken as informative values only.

Methods
X-ray fluorescence spectrometry
XRF-measurements were performed using a sequential wavelength-dispersive
XRF-Spectrometer AXS SRS 3400 WDXRF (Bruker), equipped with a Rh-Tube. Calibration,
analysis and quantification were carried out using the software SpectraPlus V 1.5.3. Signals
were automatically corrected for interferences using the aforementioned software. The
multivariate calibration curves were developed using certified values of analogue CRMs.
CHN
All measurements were done using a CE NCS 2500 Elemental Analyzer (FISONS® Instruments).
Calibration was done using 2,5-Bis(5-tert-butyl-benzoxazol-2-yl)thiophene (C%:72.53; H%: 6.09;
N%: 6.51; O%: 7.43; S%: 7.44.) as calibration standard.
Total carbon content
Total carbon content and Organic carbon content was measured using an Automatic Carbon and
Sulphur Determinator CS 900 (ELTRA). Aliquots were weighed directly into ceramic crucibles.
Combustion was achieved in a stream of oxygen. Detection was done using an IR-cell. The device
was calibrated using pure calcium carbonate, purity > 99.5 % (Fluka, Switzerland).
Organic carbon content
Total carbon content and Organic carbon content was measured using an Automatic Carbon and
Sulphur Determinator CS 900 (ELTRA). Aliquots were weighed directly into ceramic crucibles.
Combustion was achieved in a stream of oxygen. Detection was done using infrared spectrometry.
For the determination of the organic carbon content the solid samples were acidified with 1 % HCl
solution in order to destroy inorganic carbon prior to the measurements.
Mercury
Hg was measured by cold vapor atomic absorption spectrometry (CVAAS) using an AMA 245
device (ELTRA). Calibration was obtained using a Carlo Erba Hg-Standard for AAS (N° 497551)
in 2.5 % HCl: for calibration.
Results
The mean values of the observed concentrations are shown below. It should be highlighted
that these results are not certified values and are informative only.

BCR-032

Analyte Unit Average Standard deviation Replicates

Si (1) g / 100 g < 0.02 4

(1)
Al g / 100 g < 0.03 4
Ca (1) g / 100 g 27.71 0.09 4
K (1) g / 100 g < 0.04 4
(1)
Fe g / 100 g < 0.04 4
(1)
Mg g / 100 g 0.24 0.00 4
(1)
Ti mg / kg < 12 4
P (1) mg / kg 107 590 170 4
Pb (1) mg / kg 5.8 1.3 4
(1)
Zn mg / kg 164.0 1.9 4
(1)
Cu mg / kg <2 4
Ni (1) mg / kg 39.5 2.0 4
Mn (1) mg / kg 2 2
Cr (1) mg / kg 119.5 1.0 4
(1)
Na g / 100 g 0.52 0.00 4
(2)
N g / 100 g 0.018 7 0.001 5 12
C (2) g / 100 g 1.488 0.028 12
Corg (3) g / 100 g 0.98 0.06 6
(3)
Ctot g / 100 g 1.526 0.010 6

(1) determined by WDXR;

(2) determined using CHN-analyser;
(3) determined using carbon/sulphur analyser.