ISE867
ISE867
Certificate of Analysis
REFERENCE MATERIAL
General Information
In this report an overview is given of analytical data for this sample collected in our proficiency testing
program. The consensus values are calculated using a robust statistical model. With this NDA model
mean and standard deviation are calculated using all reported data when at least 8 results are left
after removal of reported 'lower than' (<) and 0 (= zero) values. No outliers are removed.
This report is divided into three sections: Consensus Values, Indicative Values and Values for
Information. The division is made on the reliability of the data. Consensus Values are based on at
least 16 results while the coefficient of variation is smaller than 25 %. Indicative Values are based on
at least 8 and less than 16 results or a coefficient of variation between 25 % and 50 %. Other values,
based on less than 8 results or a coefficient of variation higher than 50 %, are given for information
only.
In the section with Consensus Values the following parameters are given: mean, standard deviation,
coefficient of variation, number of results, median and MAD (Median of Absolute Deviation). The
confidence limits (at 95 % probabilty) are calculated for these determinands.
In the section with Indicative Values the following parameters are given: mean, standard deviation,
coefficient of variation, number of results, median and MAD.
In the section with Information Values the following parameters are given: median, MAD and number
of results. For determinands which have at least 5 results reported as smaller than (<) the median of
these ‘smaller than results’ is calculated. In some cases this median of ‘<’ values is much smaller than
median and mean of the indicative values. This may be caused by a too opmistic (too low) value for
the detection limit reported by a (small) majority of participating laboratories who report ‘<’-values.
All values, expressed on a weight basis (kg or %), are reported in ovendry (105 °C) material. Moisture
is reported in the material as received.
Sample information
WEPAL reference materials are from natural sources only. There is no spiking, mixing or other
alterations of the samples. For sample preparation the ISE samples are dried at 40 oC and milled to
pass a 0.5 mm sieve.
This ISE sample 867 of Forrest sandy soil from Netherlands is prepared for the WEPAL proficiency
programs. The sample is used in 5 periods (or rounds). The results on which the values in this report
are based were taken from the periods given in the following table.
1
Consensus Values ISE 867
Method: Real totals
Element Unit Mean Std.Dev. CV % N Median MAD 95 % confidence limits
Al g/kg 10.4 0.91 8.8 90 10.3 0.63 10.20 - 10.58
As mg/kg 4.51 0.716 15.9 64 4.59 0.498 4.33 - 4.69
Ba mg/kg 128 12.5 9.8 78 128 8.5 125.6 - 131.2
Br mg/kg 24.2 2.24 9.2 39 23.9 1.60 23.5 - 24.9
C - elementary g/kg 53.3 6.20 11.6 93 53.7 4.30 52.0 - 54.6
Ca g/kg 0.414 0.0951 23.0 78 0.415 0.0650 0.393 - 0.435
Cd mg/kg 0.272 0.0354 13.0 37 0.280 0.0260 0.260 - 0.283
Ce mg/kg 17.2 4.17 24.2 39 17.3 2.90 15.9 - 18.6
Co mg/kg 1.49 0.370 24.9 50 1.50 0.257 1.38 - 1.59
Cr mg/kg 81.9 9.83 12.0 94 82.5 6.90 79.9 - 83.9
Cu mg/kg 9.81 1.933 19.7 81 9.83 1.340 9.38 - 10.2
Fe g/kg 7.04 0.593 8.4 98 7.08 0.410 6.92 - 7.16
Hg µg/kg 51.2 7.46 14.6 53 52.2 5.18 49.2 - 53.3
K mg/kg 5250 400 7.6 96 5230 285 5170 - 5330
La mg/kg 8.20 1.935 23.6 39 8.40 1.320 7.57 - 8.82
Li mg/kg 9.33 0.773 8.3 20 9.16 0.516 8.97 - 9.69
Mg mg/kg 340 69.4 20.4 65 340 47.6 323 - 357
Mn mg/kg 55.5 8.49 15.3 81 55.1 5.90 53.7 - 57.4
Mo mg/kg 4.58 0.767 16.8 59 4.65 0.550 4.38 - 4.78
N - elementary g/kg 1.71 0.228 13.3 194 1.71 0.157 1.675 - 1.740
Na mg/kg 1360 253 18.7 76 1340 181 1300 - 1410
Nb mg/kg 3.87 0.932 24.1 35 4.10 0.700 3.55 - 4.19
Ni mg/kg 25.8 4.61 17.8 88 26.5 3.15 24.8 - 26.8
P mg/kg 175 31.9 18.3 71 179 22.1 167 - 182
Pb mg/kg 19.6 2.55 13.0 84 19.7 1.80 19.0 - 20.1
Rb mg/kg 24.7 1.97 8.0 62 24.7 1.30 24.2 - 25.2
Sb mg/kg 0.796 0.1971 24.7 28 0.788 0.1325 0.720 - 0.873
Si g/kg 403 6.6 1.6 71 403 4.8 401.6 - 404.7
Sr mg/kg 21.6 2.37 10.9 69 21.4 1.60 21.1 - 22.2
Th mg/kg 3.11 0.546 17.5 33 3.10 0.400 2.92 - 3.31
Ti mg/kg 1090 107 9.8 83 1100 75 1064 - 1111
Tl mg/kg 0.171 0.0273 15.9 19 0.170 0.0200 0.158 - 0.185
U mg/kg 0.994 0.2461 24.8 26 0.990 0.1620 0.894 - 1.09
V mg/kg 14.3 2.20 15.4 73 14.5 1.50 13.8 - 14.8
Y mg/kg 6.64 1.156 17.4 39 6.80 0.800 6.27 - 7.02
Zr mg/kg 216 20.5 9.5 58 216 14.0 210 - 221
2
Consensus Values ISE 867
Method: Acid extractable (So-called totals)
Element Unit Mean Std.Dev. CV % N Median MAD 95 % confidence limits
Al g/kg 3.11 0.728 23.4 48 3.22 0.510 2.90 - 3.33
As mg/kg 3.66 0.520 14.2 57 3.76 0.357 3.53 - 3.80
Ba mg/kg 10.9 1.94 17.8 41 11.4 1.40 10.3 - 11.5
Cd mg/kg 0.269 0.0441 16.4 74 0.270 0.0310 0.258 - 0.279
Co mg/kg 1.32 0.297 22.4 61 1.30 0.200 1.25 - 1.40
Cr mg/kg 65.7 9.42 14.3 103 64.9 6.65 63.9 - 67.6
Cu mg/kg 8.47 0.986 11.6 115 8.54 0.694 8.29 - 8.65
Fe g/kg 6.29 0.811 12.9 71 6.25 0.570 6.10 - 6.48
Hg µg/kg 52.6 10.08 19.2 43 52.3 7.15 49.5 - 55.7
Mn mg/kg 35.9 6.82 19.0 75 35.8 4.60 34.3 - 37.4
Mo mg/kg 4.75 0.624 13.1 45 4.71 0.452 4.56 - 4.94
N g/kg 1.56 0.199 12.7 115 1.56 0.140 1.523 - 1.596
Ni mg/kg 25.4 2.74 10.8 101 25.1 1.90 24.9 - 26.0
P mg/kg 148 25.8 17.4 81 150 18.0 142 - 153
Pb mg/kg 16.8 1.55 9.2 107 16.7 1.06 16.50 - 17.10
S mg/kg 232 33.4 14.4 47 241 24.0 222 - 242
Sn mg/kg 0.900 0.1545 17.2 20 0.924 0.1100 0.828 - 0.972
V mg/kg 9.65 1.190 12.3 47 9.70 0.800 9.30 - 10.00
Zn mg/kg 8.52 1.579 18.5 93 8.70 1.110 8.20 - 8.85
3
Consensus Values ISE 867
Method: Aqua Regia (ISO 11466) (cont.)
Element Unit Mean Std.Dev. CV % N Median MAD 95 % confidence limits
P mg/kg 144 12.0 8.3 89 144 8.0 141.8 - 146.8
Pb mg/kg 16.7 1.61 9.6 128 16.7 1.11 16.45 - 17.01
S mg/kg 222 17.1 7.7 68 223 11.5 218 - 226
Sb mg/kg 0.454 0.0560 12.3 30 0.469 0.0412 0.433 - 0.475
Se mg/kg 0.358 0.0683 19.1 41 0.360 0.0480 0.337 - 0.380
Sn mg/kg 0.797 0.1171 14.7 26 0.824 0.0845 0.750 - 0.844
Ti mg/kg 131 31.8 24.3 31 130 20.0 119 - 143
U mg/kg 0.287 0.0223 7.8 20 0.286 0.0155 0.276 - 0.297
V mg/kg 9.31 1.010 10.8 59 9.40 0.700 9.05 - 9.58
Zn mg/kg 8.38 1.185 14.2 132 8.52 0.825 8.17 - 8.58
4
Consensus Values ISE 867
Method: Soil characteristics
Element Unit Mean Std.Dev. CV % N Median MAD 95 % confidence limits
C - org others (W&B a.o.) g/kg 49.8 8.11 16.3 189 50.0 5.70 48.7 - 51.0
EC-SC (ISO 11265) mS/m 11.0 2.45 22.2 143 11.1 1.70 10.6 - 11.4
Fraction < 63 µm % 28.2 5.21 18.4 78 28.1 3.58 27.1 - 29.4
Fraction > 63 µm % 71.3 5.46 7.7 68 71.4 3.84 70.0 - 72.7
Org.matter (L.O.I.) % 8.85 0.415 4.7 132 8.88 0.286 8.77 - 8.92
pH - CaCl2 ... 3.62 0.188 5.2 147 3.63 0.130 3.589 - 3.650
pH - H2O ... 3.90 0.171 4.4 354 3.92 0.120 3.885 - 3.921
pH - KCl ... 3.59 0.204 5.7 156 3.59 0.140 3.554 - 3.619
TC=Total C (org.+inorg.) g/kg 52.9 4.92 9.3 137 52.7 3.40 52.1 - 53.7
TOC=Total Org. C g/kg 50.9 5.27 10.3 128 50.5 3.65 50.0 - 51.8
Method: Mehlich-3
Element Unit Mean Std.Dev. CV % N Median MAD 95 % confidence limits
Al mg/kg 1060 172 16.2 42 1040 119 1010 - 1120
K mg/kg 36.9 7.25 19.6 83 37.5 5.01 35.3 - 38.5
Mn mg/kg 7.88 1.658 21.0 68 7.94 1.145 7.48 - 8.28
Zn mg/kg 2.30 0.573 24.9 68 2.32 0.390 2.16 - 2.43
5
Consensus Values ISE 867
Method: Extraction with 0.01M CaCl2 - 0.005M DTPA 1:10 (w/v)
Element Unit Mean Std.Dev. CV % N Median MAD 95 % confidence limits
Fe mg/kg 669 156.1 23.3 50 657 105.8 625 - 713
6
Indicative Values ISE 867
Method: Real totals Results smaller than (<)
Element Unit Mean Std.Dev. CV % N Median MAD Median of < N
Be mg/kg 0.213 0.0859 40.4 14 0.204 0.0550 0.750 10
Ga mg/kg 3.87 1.313 33.9 40 4.00 0.905 7.50 8
I mg/kg 7.19 2.168 30.2 16 7.45 1.495
Nd mg/kg 6.96 2.535 36.4 26 7.12 1.670 25.00 6
S mg/kg 266 71.1 26.8 66 278 50.4 1000 7
Sn mg/kg 1.44 0.544 37.7 25 1.60 0.400 2.00 21
W mg/kg 0.966 0.2745 28.4 16 0.980 0.2000 3.000 8
Zn mg/kg 10.7 2.75 25.7 81 11.0 1.90 20.0 12
7
Indicative Values ISE 867
Method: Extraction with 0.01M CaCl2 1:10 (cont.)
Element Unit Mean Std.Dev. CV % N Median MAD
N total soluble mg/kg 48.0 8.45 17.6 10 49.5 6.39
Na mg/kg 12.3 3.11 25.3 16 13.2 2.32
Zn µg/kg 1620 164 10.1 10 1630 117
Method: Pot. CEC using 1M NH4-acetate at pH=7 Results smaller than (<)
Element Unit Mean Std.Dev. CV % N Median MAD Median of < N
CEC cmol+/kg 12.7 3.25 25.6 128 12.8 2.22
K cmol+/kg 0.0949 0.0276 29.0 178 0.1000 0.0195 0.1300 5
Mg cmol+/kg 0.0947 0.0419 44.2 167 0.1000 0.0300 0.0500 8
Na cmol+/kg 0.0579 0.0286 49.3 135 0.0600 0.0200 0.0750 10
Method: Pot. CEC using 1M or 0.1M BaCl2-TEA at pH=8.1 (ISO 13536 OR BZE)
Element Unit Mean Std.Dev. CV % N Median MAD
CEC cmol+/kg 22.5 5.09 22.7 13 23.0 3.37
8
Indicative Values ISE 867
Method: Act. CEC using 0.1M BaCl2 (UNEP-UN/EC 91065A)
Element Unit Mean Std.Dev. CV % N Median MAD
Al cmol+/kg 2.26 0.147 6.5 12 2.27 0.096
Ca cmol+/kg 0.179 0.0294 16.4 14 0.176 0.0210
CEC cmol+/kg 5.48 0.319 5.8 12 5.45 0.222
Fe cmol+/kg 2.59 0.357 13.8 13 2.61 0.250
K cmol+/kg 0.0876 0.0067 7.6 14 0.0865 0.0045
Mg cmol+/kg 0.0802 0.0115 14.3 13 0.0830 0.0080
Mn cmol+/kg 0.0255 0.0049 19.4 10 0.0265 0.0035
Na cmol+/kg 0.0499 0.0070 14.1 14 0.0510 0.0045
9
Indicative Values ISE 867
Method: UK Soil Methods
Element Unit Mean Std.Dev. CV % N Median MAD
Mg - NH4NO3 (1/5) mg/l 15.2 4.24 27.9 52 15.2 2.80
10
Informative Values ISE 867
Method: Real totals Results smaller than (<)
Element Unit Median MAD N Median of < N
Ag mg/kg 0.925 0.7800 4 2.000 14
B mg/kg 15.0 2.00 5
Bi mg/kg 2.20 1.400 6 3.00 16
Cs mg/kg 1.49 0.560 16 3.00 6
F mg/kg 768 - 1 50.0 5
Ge mg/kg 1.000 0.3000 5 3.000 7
Sc mg/kg 1.43 0.595 18 10.00 8
Se mg/kg 0.681 0.3805 14 2.000 13
11
Informative Values ISE 867
Method: Aqua Regia (ISO 11466) Results smaller than (<) (cont.)
Element Unit Median MAD N Median of < N
Ce mg/kg 10.5 0.78 6
Ga mg/kg 1.81 0.100 3
I mg/kg 6.03 - 1
N g/kg 2.30 - 1
Na mg/kg 35.0 13.82 60 50.0 12
Nd mg/kg 4.54 0.217 4
Rb mg/kg 4.03 0.815 4
Sc mg/kg 0.310 0.0800 6
Si g/kg 200 199.7 2
Te mg/kg 0.0100 0.0020 2
Th mg/kg 0.309 0.0450 5
Y mg/kg 0.842 0.0185 2
Zr mg/kg 7.78 - 1
Method: Extraction with 0.01M CaCl2 1:10 Results smaller than (<)
Element Unit Median MAD N Median of < N
B µg/kg 265 101.8 8
Cd µg/kg 0.200 - 1
Co µg/kg 41.5 5.47 7
Cr µg/kg 0.310 - 1
Ni µg/kg 0.460 - 1
P mg/kg 0.470 0.2600 17 0.300 5
Pb µg/kg 12.9 - 1
SO4 mg/kg 55.9 24.22 3
12
Informative Values ISE 867
Method: Digestion with conc. HNO3 + conc. HCl + H2O2 (UNEP-UN/EC 91075A)
Element Unit Median MAD N
Al g/kg 4.73 - 1
As mg/kg 2.94 - 1
Ca g/kg 0.0930 - 1
Cd mg/kg 0.236 0.0355 2
Co mg/kg 1.51 0.180 3
Cr mg/kg 52.4 3.70 3
Cu mg/kg 9.44 0.240 3
Fe g/kg 7.08 2.562 2
Hg mg/kg 0.240 - 1
K mg/kg 433 - 1
Mg mg/kg 200 - 1
Mn mg/kg 29.0 10.00 3
Mo mg/kg 2.21 - 1
Na mg/kg 149 - 1
Ni mg/kg 22.0 5.78 3
P mg/kg 200 - 1
Pb mg/kg 16.5 2.03 3
S mg/kg 261 - 1
V mg/kg 9.92 - 1
Zn mg/kg 7.21 1.595 2
Method: Pot. CEC using 1M NH4-acetate at pH=7 Results smaller than (<)
Element Unit Median MAD N Median of < N
Al cmol+/kg 0.741 0.4055 6
Ca cmol+/kg 0.185 0.0910 152 0.500 11
Method: Pot. CEC using 1M or 0.1M BaCl2-TEA at pH=8.1 (ISO 13536 OR BZE)
Element Unit Median MAD N
Al cmol+/kg 3.54 0.250 3
Ca cmol+/kg 0.150 0.0100 5
K cmol+/kg 0.110 0.0290 7
Mg cmol+/kg 0.100 0.0200 6
Na cmol+/kg 0.130 0.0100 7
13
Informative Values ISE 867
Method: Pot. CEC using 1M NH4Cl (BZE)
Element Unit Median MAD N
H cmol+/kg 0.310 0.1750 12
14
Informative Values ISE 867
Method: Water soluble 1:10 (w/v) (EN-12457-4)
Element Unit Median MAD N
Cl mg/kg 43.4 20.40 5
F mg/kg 13.6 13.39 2
N - NO3 (as N) mg/kg 2.25 0.750 4
Method: Extraction with dilute nitric acid (0.43 Mol/l) ISO 17586
Element Unit Median MAD N
Cd mg/kg 199 - 1
Fe g/kg 0.190 - 1
Mn mg/kg 31.0 - 1
Pb mg/kg 178 - 1
15