CERTIFICATE OF ANALYSIS FLX-CRM 113 Cement...2 O 3 5.14 0.07 NIST 1880B CaO 64.61 0.25 SI unit kg/kg...

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FLUXANA

CERTIFICATE OF ANALYSIS

FLX-CRM 113 Cement

Mass fraction in % Certified value1) Uncertainty2) Traceable to Al2O3 5.06 0.07 NIST 1880B

CaO 63.63 0.25 SI unit kg/kg

Cr2O3 0.007 0.002 NIST 1880B

Fe2O3 2.75 0.03 NIST 1880B

K2O 0.619 0.025 NIST 1880B

MgO 2.49 0.06 NIST 1880B

Mn2O3 0.233 0.020 NIST 1880B

Na2O 0.092 0.027 NIST 1880B

P2O5 0.135 0.003 NIST 1880B

SiO2 20.98 0.09 SI unit kg/kg

SO3 total 2.47 0.12 NIST 1880B

SO42- as SO3 2.40 0.15 SI unit kg/kg

SrO 0.064 0.019 NIST 1880B

TiO2 0.231 0.013 NIST 1880B

ZnO 0.030 0.002 NIST 1880B

LOI 1.53 0.08 not certified, info only

S2- 0.137 0.019 not certified, info only

1) Certified value traceable to cement NIST 1880B or SI unit kg/kg based on original sample material. 2) Expanded uncertainty UCRM calculated for a confidence interval of 95% (k=2) based on a combined

uncertainty of characterization, homogeneity and long term stability.

The sum of all oxides is 100.31%. This includes SO3 total and LOI and excludes SO42- as SO3 and S2-. Bedburg-Hau, 01.06.2015 Responsible Reference Materials Statistics and Report Dr. Barbara Schäfer Dr. Rainer Schramm

mailto:[email protected]://www.fluxana.com/



Description of the CRM This reference material is an industrial product and was taken directly from the production stream. The complete batch was sealed into 30g bottles. This material is normally used as cement for constructions. Intended use Calibration and control sample for x-ray fluorescence (XRF) analysis. Instructions for the correct use of the CRM This material is moisture sensitive. It can only be used without any sample pretreatment if the original seal is intact. After opening the material has to be sealed again as soon as possible to avoid any change. Otherwise it has to be ignited for minimum 1 hour at 950°C prior to use. The ignition process must result in a constant weight. The ignited material must be stored in a desiccator not longer than 24h, then reignition might be necessary. The minimum sample quantity for analysis should be 1.0g to be in agreement with the stated uncertainties. For XRF use, ignited samples should be prepared as a fused bead, e.g. in accordance with ISO 29581-2:2010. The following table contains the certified values concoriginal recalculated to ignited sample values concignited as obtained directly from, e.g., a fused bead by the following formula:

𝑐𝑜𝑛𝑐𝑖𝑔𝑛𝑖𝑡𝑒𝑑 =𝑐𝑜𝑛𝑐𝑜𝑟𝑖𝑔𝑖𝑛𝑎𝑙 ∗ 𝑆𝑢𝑚

𝑆𝑢𝑚 − 𝐿𝑂𝐼

FLX-CRM 113 Certified values for ignited sample

mass% concignited UCRM Traceable to

Al2O3 5.14 0.07 NIST 1880B


Cr2O3 0.007 0.002 NIST 1880B

Fe2O3 2.80 0.03 NIST 1880B

K2O 0.628 0.026 NIST 1880B

MgO 2.52 0.06 NIST 1880B

Mn2O3 0.237 0.021 NIST 1880B

Na2O 0.094 0.027 NIST 1880B

P2O5 0.137 0.003 NIST 1880B


SO3 total 2.51 0.13 NIST 1880B

SO42- as SO3

SrO 0.065 0.019 NIST 1880B

TiO2 0.234 0.013 NIST 1880B

ZnO 0.030 0.002 NIST 1880B

LOI

S2-

Sum 100.31




Expiration of Certification This certificate is valid, within the uncertainty specified, until 31.05.2025, provided the CRM is handled in accordance with instructions given in this certificate. The certification is nullified if the CRM is damaged, contaminated, or otherwise modified. Hazardous situation For this material an actual MSDS is available. Level of homogeneity In accordance with ISO Guide 35: 2006 a homogeneity study was performed. A one-way ANOVA was used to calculate the batch inhomogeneity 𝑢2𝑏𝑏 .

𝑢2𝑏𝑏 =𝑀𝑆𝑎𝑚𝑜𝑛𝑔 − 𝑀𝑆𝑤𝑖𝑡ℎ𝑖𝑛

𝑛

𝑀𝑆𝑎𝑚𝑜𝑛𝑔 quadratic mean of the results of homogeneity between bottle

𝑀𝑆𝑤𝑖𝑡ℎ𝑖𝑛 quadratic mean of the results of homogeneity within bottle 𝑛 number of measurements per bottle

Stability In accordance with ISO Guide 35: 2006 a stability study was performed. As a result the material was considered as stable. The uncertainty of long term stability u²lts was calculated. Total expanded uncertainty The total expanded uncertainty UCRM for a confidence interval of 95% (k=2) was calculated by taking into account the uncertainty from characterization 𝑢2𝑐ℎ𝑎𝑟, from inhomogeneity 𝑢

2𝑏𝑏 and long term stability

𝑢2𝑙𝑡𝑠 with the following formula:

𝑈𝐶𝑅𝑀 = 𝑘 × √𝑢2𝑐ℎ𝑎𝑟 + 𝑢2𝑏𝑏 + 𝑢2𝑙𝑡𝑠 Traceability The analytical work performed to assess this material was carried out by the FLUXANA laboratory, which works under DIN EN ISO/IEC 17025 accreditation. All of the results derived as part of this testing program have traceability to NIST 1880B from NIST and some additionally to the SI unit kg. Methods used In accordance with ISO Guide 34, we use the approach “measurement by a single (primary) method in a single laboratory”. An example for this approach is also found in DIN ISO 13528:2009-01 chapter 5.4. Using




this approach, samples of the test material that is to be the new reference material are prepared first. They are tested along with CRMs or synthetic RMs using a suitable method. The assigned values XCRM and their uncertainties UCRM are then derived from a calibration against the certified reference values of the CRMs. The error of the calibration used can be neglected because only the differences in the results between the new reference material and the CRM or synthetic RM are part of the evaluation. CRM used: NIST 1880B Synthetic RMs made from pure chemicals by weighing Measurement method used: ISO 29581-2:2010-03 Further information The following table lists all results obtained for this sample material. Values in bold represent the results with the smallest uncertainty; i.e., those used for the certification. Users who need all values traceable to a NIST CRM are provided with all results in the following table. However in comparison with the values traceable to the SI unit, they show a higher uncertainty. For comparison with the certified values, the results of an independently performed proficiency test are also given. A detailed report is available at www.fluxana.com.

FLX-CRM 113 Traceable to Traceable to For Comparison

NIST 1880B SI unit kg/kg results of PT

mass% XCRM UCRM XCRM UCRM XPT UPT

Al2O3 5.06 0.07 5.04 0.05

CaO 63.62 0.47 63.63 0.25 63.68 0.27

Cr2O3 0.007 0.002 0.008 0.001

Fe2O3 2.76 0.03 2.76 0.03

K2O 0.619 0.025 0.586 0.028

MgO 2.49 0.06 2.45 0.03

Mn2O3 0.233 0.020 0.22 0.02

Na2O 0.092 0.027 0.106 0.031

P2O5 0.135 0.003 0.137 0.007

SiO2 20.99 0.37 20.98 0.09 21.10 0.14

SO3 total 2.47 0.12 2.55 0.07

SO42- as SO3 2.40 0.15 2.40 0.151)

SrO 0.064 0.019 0.063 0.01

TiO2 0.231 0.013 0.231 0.01

ZnO 0.030 0.002 0.028 0.004

LOI 1.58 0.08 1.53 0.081) 1.47 0.06

S2- 0.137 0.019

Sum (w/o SO42-+S2-) 100.36 100.43

1) UCRM taken from the calculations based on NIST 1880B. This certificate is in conformance with ISO Guide 31:2000.

mailto:[email protected]://www.fluxana.com/http://www.fluxana.com/



FLUXANA


FLX-CRM 114 Cement

Mass fraction in % Certified value1) Uncertainty2) Traceable to Al2O3 6.94 0.08 NIST 1881A


Cr2O3 0.005 0.003 NIST 1881A

Fe2O3 1.37 0.15 NIST 1881A

K2O 0.954 0.160 NIST 1881A

MgO 4.93 0.21 NIST 1881A

Mn2O3 0.154 0.012 NIST 1881A

Na2O 0.277 0.044 NIST 1881A

P2O5 0.027 0.008 NIST 1881A


SO3 total 4.07 0.20 not certified, info only


SrO 0.108 0.027 NIST 1881A

TiO2 0.525 0.011 NIST 1881A

ZnO 0.022 0.003 NIST 1881A



1) Certified value traceable to cement NIST 1881A or SI unit kg/kg based on original sample material. 2) Expanded uncertainty UCRM calculated for a confidence interval of 95% (k=2) based on a combined

uncertainty of characterization, homogeneity and long term stability. The sum of all oxides is 100.55%. This includes SO3 total and LOI and excludes SO42- as SO3 and S2-. Bedburg-Hau, 01.06.2015 Responsible Reference Materials Statistics and Report Dr. Barbara Schäfer Dr. Rainer Schramm









Al2O3 7.03 0.09 NIST 1881A


Cr2O3 0.005 0.003 NIST 1881A

Fe2O3 1.39 0.15 NIST 1881A

K2O 0.966 0.162 NIST 1881A

MgO 4.99 0.22 NIST 1881A

Mn2O3 0.156 0.012 NIST 1881A

Na2O 0.281 0.045 NIST 1881A

P2O5 0.028 0.008 NIST 1881A


SO3 total

SO42- as SO3

SrO 0.109 0.028 NIST 1881A

TiO2 0.532 0.011 NIST 1881A

ZnO 0.023 0.003 NIST 1881A

LOI

S2-






𝑛






𝑈𝐶𝑅𝑀 = 𝑘 × √𝑢2𝑐ℎ𝑎𝑟 + 𝑢2𝑏𝑏 + 𝑢2𝑙𝑡𝑠 Traceability The analytical work performed to assess this material was carried out by the FLUXANA laboratory, which works under DIN EN ISO/IEC 17025 accreditation. All of the results derived as part of this testing program have traceability to NIST 1881A from NIST and some additionally to the SI unit kg. Methods used In accordance with ISO Guide 34, we use the approach “measurement by a single (primary) method in a single laboratory”. An example for this approach is also found in DIN ISO 13528:2009-01 chapter 5.4. Using




this approach, samples of the test material that is to be the new reference material are prepared first. They are tested along with CRMs or synthetic RMs using a suitable method. The assigned values XCRM and their uncertainties UCRM are then derived from a calibration against the certified reference values of the CRMs. The error of the calibration used can be neglected because only the differences in the results between the new reference material and the CRM or synthetic RM are part of the evaluation. CRM used: NIST 1881A Synthetic RMs made from pure chemicals by weighing Measurement method used: ISO 29581-2:2010-03 Further information The following table lists all results obtained for this sample material. Values in bold represent the results with the smallest uncertainty; i.e., those used for the certification. Users who need all values traceable to a NIST CRM are provided with all results in the following table. However in comparison with the values traceable to the SI unit, they show a higher uncertainty. For comparison with the certified values, the results of an independently performed proficiency test are also given. A detailed report is available at www.fluxana.com.


NIST 1881A SI unit kg/kg results of PT


Al2O3 6.94 0.08 6.94 0.09

CaO 51.35 0.37 51.29 0.14 51.19 0.29

Cr2O3 0.005 0.003 0.009 0.002

Fe2O3 1.37 0.15 1.44 0.03

K2O 0.954 0.160 0.903 0.031

MgO 4.93 0.21 4.84 0.05

Mn2O3 0.154 0.012 0.148 0.014

Na2O 0.277 0.044 0.260 0.031

P2O5 0.027 0.008 0.024 0.004

SiO2 28.66 0.30 28.61 0.26 28.70 0.16

SO3 total 4.07 0.20

SO42- as SO3 2.581) 0.02 2.50 0.023)

SrO 0.108 0.027 0.102 0.013

TiO2 0.525 0.011 0.518 0.014

ZnO 0.022 0.003 0.022 0.005

LOI 1.382) 0.18 1.28 0.183) 1.02 0.06

S2- 0.676 0.182

Sum (w/o SO42-+S2-) 100.18

1) Traceable to NIST 1880B. 2) Traceable to NIST 1888B. 3) UCRM taken from calculations based on NIST CRM. This certificate is in conformance with ISO Guide 31:2000.




FLUXANA


FLX-CRM 115 Cement



Cr2O3 0.004 0.004 NIST 1881A

Fe2O3 0.972 0.143 NIST 1881A

K2O 0.612 0.087 NIST 1881A

MgO 2.93 0.12 NIST 1881A

Mn2O3 0.214 0.035 NIST 1881A

Na2O 0.194 0.050 NIST 1881A

P2O5 0.073 0.006 NIST 1881A




SrO 0.117 0.014 NIST 1881A

TiO2 0.610 0.018 NIST 1881A

ZnO 0.008 0.004 NIST 1881A














Al2O3 8.26 0.08 NIST 1881A


Cr2O3 0.004 0.004 NIST 1881A

Fe2O3 0.987 0.145 NIST 1881A

K2O 0.622 0.088 NIST 1881A

MgO 2.98 0.13 NIST 1881A

Mn2O3 0.217 0.035 NIST 1881A

Na2O 0.197 0.051 NIST 1881A

P2O5 0.074 0.007 NIST 1881A


SO3 total

SO42- as SO3

SrO 0.119 0.014 NIST 1881A

TiO2 0.620 0.018 NIST 1881A

ZnO 0.008 0.004 NIST 1881A

LOI

S2-






𝑛














Al2O3 8.13 0.08 8.12 0.08

CaO 54.05 0.41 53.93 0.22 53.78 0.28

Cr2O3 0.004 0.004 0.008 0.003

Fe2O3 0.972 0.143 1.06 0.02

K2O 0.612 0.087 0.594 0.028

MgO 2.93 0.12 2.87 0.04

Mn2O3 0.214 0.035 0.200 0.021

Na2O 0.194 0.050 0.179 0.027

P2O5 0.073 0.006 0.071 0.007

SiO2 27.39 0.16 27.29 0.06 27.32 0.19

SO3 total 3.90 0.26

SO42- as SO3 2.491) 0.02 2.41 0.023)

SrO 0.117 0.014 0.11 0.013

TiO2 0.610 0.018 0.597 0.016

ZnO 0.008 0.004 0.01 0.002

LOI 1.672) 0.08 1.56 0.083) 1.32 0.06

S2- 0.611 0.340

Sum (w/o SO42-+S2-) 100.13





FLUXANA


FLX-CRM 116 Cement



Cr2O3 0.005 0.002 NIST 1881A

Fe2O3 0.86 0.12 NIST 1881A

K2O 0.693 0.129 NIST 1881A

MgO 4.47 0.20 NIST 1881A

Mn2O3 0.238 0.035 NIST 1881A

Na2O 0.201 0.049 NIST 1881A

P2O5 0.034 0.007 NIST 1881A




SrO 0.091 0.036 NIST 1881A

TiO2 0.690 0.011 NIST 1881A

ZnO 0.015 0.004 NIST 1881A

LOI -0.394 0.315 not certified, info only













Al2O3 9.08 0.13 NIST 1881A


Cr2O3 0.005 0.002 NIST 1881A

Fe2O3 0.860 0.123 NIST 1881A

K2O 0.690 0.129 NIST 1881A

MgO 4.45 0.20 NIST 1881A

Mn2O3 0.237 0.035 NIST 1881A

Na2O 0.200 0.049 NIST 1881A

P2O5 0.034 0.007 NIST 1881A


SO3 total

SO42- as SO3

SrO 0.091 0.036 NIST 1881A

TiO2 0.687 0.011 NIST 1881A

ZnO 0.015 0.004 NIST 1881A

LOI

S2-






𝑛














Al2O3 9.11 0.13 9.06 0.10

CaO 50.05 0.35 50.05 0.08 49.86 0.32

Cr2O3 0.005 0.002 0.007 0.003

Fe2O3 0.864 0.123 0.966 0.023

K2O 0.693 0.129 0.662 0.028

MgO 4.47 0.20 4.40 0.05

Mn2O3 0.238 0.035 0.221 0.023

Na2O 0.201 0.049 0.208 0.036

P2O5 0.034 0.007 0.029 0.004

SiO2 30.88 0.25 30.81 0.20 30.71 0.18

SO3 total 3.14 0.24

SO42- as SO3 1.301) 0.020 1.22 0.023)

SrO 0.091 0.036 0.081 0.012

TiO2 0.690 0.011 0.683 0.018

ZnO 0.015 0.004 0.016 0.003

LOI -0.3372) 0.455 -0.394 0.3153) -0.164 0.175

S2- 0.737 0.249

Sum (w/o SO42-+S2-) 99.89





FLUXANA


FLX-CRM 117 Cement



Cr2O3 0.004 0.005 NIST 1881A

Fe2O3 1.37 0.16 NIST 1881A

K2O 0.916 0.113 NIST 1881A

MgO 2.95 0.17 NIST 1881A

Mn2O3 0.193 0.031 NIST 1881A

Na2O 0.223 0.046 NIST 1881A

P2O5 0.035 0.010 NIST 1881A




SrO 0.098 0.018 NIST 1881A

TiO2 0.564 0.012 NIST 1881A

ZnO 0.024 0.003 NIST 1881A














Al2O3 7.72 0.09 NIST 1881A


Cr2O3 0.004 0.005 NIST 1881A

Fe2O3 1.37 0.16 NIST 1881A

K2O 0.920 0.113 NIST 1881A

MgO 2.96 0.17 NIST 1881A

Mn2O3 0.194 0.031 NIST 1881A

Na2O 0.224 0.046 NIST 1881A

P2O5 0.035 0.010 NIST 1881A


SO3 total

SO42- as SO3

SrO 0.099 0.018 NIST 1881A

TiO2 0.567 0.012 NIST 1881A

ZnO 0.024 0.003 NIST 1881A

LOI

S2-






𝑛














Al2O3 7.68 0.09 7.68 0.10

CaO 54.34 0.36 54.22 0.11 54.26 0.30

Cr2O3 0.004 0.005 0.007 0.003

Fe2O3 1.37 0.16 1.46 0.02

K2O 0.916 0.113 0.871 0.038

MgO 2.95 0.17 2.88 0.05

Mn2O3 0.193 0.031 0.181 0.017

Na2O 0.223 0.046 0.205 0.025

P2O5 0.035 0.010 0.030 0.005

SiO2 28.14 0.17 28.05 0.09 28.12 0.15

SO3 total 3.49 0.14

SO42- as SO3 1.871) 0.03 1.803) 0.03

SrO 0.098 0.018 0.092 0.013

TiO2 0.564 0.012 0.556 0.016

ZnO 0.024 0.003 0.023 0.004

LOI 0.4022) 0.251 0.3453) 0.251 0.215 0.097

S2- 0.602 0.395

Sum (w/o SO42-+S2-) 100.08



FLX‐0118‐02‐COA Page 1/ 5

Tel: +49 2821 48011‐10/ Fax: +49 2821 48011‐99, e‐mail: [email protected], web: www.fluxana.com, FLUXANA® GmbH & Co. KG, Borschelstr.3, 47551 Bedburg‐Hau Germany, GM Dr. R. Schramm, reg.in Kleve HRA 2935, personal liability FLUXANA Verwaltungs‐GmbH Bedburg‐Hau, reg.in Kleve HRB 8211, FLUXANA® registered trademark


FLX‐CRM 118 Cement New certificate issued July 2019

Mass fraction in % Certified value1) Uncertainty2) Traceable to Al2O3 6.94 0.09 NIST 1881A CaO 55.47 0.11 SI unit kg/kg Cr2O3 0.009 0.003 NIST 1881A Fe2O3 3.88 0.12 NIST 1881AK2O 0.983 0.030 NIST 1881A MgO 2.08 0.09 NIST 1881A Mn2O3 0.176 0.002 NIST 1881A Na2O 0.181 0.015 NIST 1881A P2O5 0.163 0.007 NIST 1881A SiO2 21.57 0.11 SI unit kg/kg SO3 total 2.97 0.06 not certified, info only SO42‐ as SO3 2.89 0.29 SI unit kg/kg SrO 0.087 0.158 NIST 1881A TiO2 0.301 0.007 NIST 1881A ZnO 0.053 0.004 NIST 1881A LOI3) 5.02 0,15 not certified, info only S2‐ 0.131 0.155 not certified, info only 1) Certified value traceable to cement NIST 1881A or SI unit kg/kg based on original sample material. 2) Expanded uncertainty UCRM calculated for a confidence interval of 95% (k=2) based on a combined

uncertainty of characterization, homogeneity and long term stability. 3) LOI is informal only and is excluded from certification because it might change over time.

The sum of all oxides is 99.88%. This includes SO3 total and LOI and excludes SO42‐ as SO3 and S2‐. Bedburg‐Hau, 26.07.2019 Responsible Reference Materials General Manager Susan Aschenbrenner Dr. Rainer Schramm



Description of the CRM This reference material is an industrial product and was taken directly from the production stream. The complete batch was sealed into 30g bottles. This material is normally used as cement for constructions. Intended use Calibration and control sample for x‐ray fluorescence (XRF) analysis. Instructions for the correct use of the CRM This material is moisture sensitive. The Material has to be dried prior to use. After opening the material has to be sealed again as soon as possible to avoid any change. Otherwise it has to be ignited for minimum 1 hour at 950°C prior to use. The ignition process must result in a constant weight. The ignited material must be stored in a desiccator not longer than 24h, then reignition might be necessary. The minimum sample quantity for analysis should be 1.0g to be in agreement with the stated uncertainties. For XRF use, ignited samples should be prepared as a fused bead, e.g. in accordance with ISO 29581‐2:2010. If the sample is used after ignition 950°C to constant mass , the ignited certified values have to be calculated, using the following formula: 𝑐𝑜𝑛𝑐 𝑐𝑜𝑛𝑐 ∗ 𝑆𝑢𝑚𝑆𝑢𝑚 𝐿𝑂𝐼



The following table contains an example of certified values concoriginal recalculated to ignited sample values concignited (LOI=5,02%) as obtained directly from, e.g., a fused bead. FLX‐CRM 118 Certified values for ignited sample mass% concignited UCRM Traceable to Al2O3 7.31 0.09 NIST 1881A CaO 58.41 0.12 SI unit kg/kg Cr2O3 0.009 0.003 NIST 1881A Fe2O3 4.08 0.13 NIST 1881A K2O 1.03 0.03 NIST 1881A MgO 2.19 0.10 NIST 1881A Mn2O3 0.186 0.002 NIST 1881A Na2O 0.191 0.015 NIST 1881A P2O5 0.171 0.007 NIST 1881A SiO2 22.72 0.11 SI unit kg/kg SO3 total 3.12 0.07 not certified, info only SO42‐ as SO3 SrO 0.092 0.166 NIST 1881A TiO2 0.317 0.007 NIST 1881A ZnO 0.056 0.004 NIST 1881A LOI S2‐ Expiration of Certification This certificate is valid, within the uncertainty specified, until 31.05.2025, provided the CRM is handled in accordance with instructions given in this certificate. The certification is nullified if the CRM is damaged, contaminated, or otherwise modified. Hazardous situation For this material an actual MSDS is available.



Level of homogeneity In accordance with ISO Guide 35: 2006 a homogeneity study was performed. A one‐way ANOVA was used to calculate the batch inhomogeneity 𝑢 .

𝑢 𝑀𝑆 𝑀𝑆𝑛

𝑀𝑆 quadratic mean of the results of homogeneity between bottle 𝑀𝑆 quadratic mean of the results of homogeneity within bottle 𝑛 number of measurements per bottle

Stability In accordance with ISO Guide 35: 2006 a stability study was performed. As a result the material was considered as stable. The uncertainty of long term stability u²lts was calculated. Total expanded uncertainty The total expanded uncertainty UCRM for a confidence interval of 95% (k=2) was calculated by taking into account the uncertainty from characterization 𝑢 , from inhomogeneity 𝑢 and long term stability 𝑢 with the following formula:

𝑈 𝑘 𝑢 𝑢 𝑢 Traceability The analytical work performed to assess this material was carried out by the FLUXANA laboratory, which works under DIN EN ISO/IEC 17025 accreditation. All of the results derived as part of this testing program have traceability to NIST 1881A from NIST and some additionally to the SI unit kg. Methods used In accordance with ISO Guide 34, we use the approach “measurement by a single (primary) method in a single laboratory”. An example for this approach is also found in DIN ISO 13528:2009‐01 chapter 5.4. Using this approach, samples of the test material that is to be the new reference material are prepared first. They are tested along with CRMs or synthetic RMs using a suitable method. The assigned values XCRM and their uncertainties UCRM are then derived from a calibration against the certified reference values of the CRMs. The error of the calibration used can be neglected because only the differences in the results between the new reference material and the CRM or synthetic RM are part of the evaluation.



CRM used: NIST 1881A Synthetic RMs made from pure chemicals by weighing Measurement method used: ISO 29581‐2:2010‐03 Further information The following table lists all results obtained for this sample material. Values in bold represent the results with the smallest uncertainty; i.e., those used for the certification. Users who need all values traceable to a NIST CRM are provided with all results in the following table. However in comparison with the values traceable to the SI unit, they show a higher uncertainty. For comparison with the certified values, the results of an independently performed proficiency test are also given. A detailed report is available at www.fluxana.com. FLX‐CRM 118 Traceable to Traceable to For Comparison NIST 1881A SI unit kg/kg results of PT mass% XCRM UCRM XCRM UCRM XPT UPT Al2O3 6.94 0.09 6.95 0.10 CaO 55.47 0.36 55.47 0.11 55.85 0.22 Cr2O3 0.009 0.003 0.011 0.002Fe2O3 3.88 0.12 3.90 0.05 K2O 0.983 0.030 0.969 0.021MgO 2.08 0.09 2.06 0.03 Mn2O3 0.176 0.002 0.178 0.007Na2O 0.181 0.015 0.169 0.025P2O5 0.163 0.007 0.161 0.003SiO2 21.54 0.18 21.57 0.11 21.60 0.14 SO3 total 2.97 0.06 SO42‐ as SO3 2.961) 0.29 2.89 0.293) 2.92 0.10SrO 0.087 0.158 0.084 0.006TiO2 0.301 0.007 0.305 0.008ZnO 0.053 0.004 0.051 0.004LOI 5.132) 0.15 5.02 0.153) 4.94 0.07 S2‐ 0.131 0.155

Sum (w/o SO42‐+S2‐) 100.19 1) Traceable to NIST 1880B. 2) Traceable to NIST 1888B. 3) UCRM taken from calculations based on NIST CRM. This certificate is in conformance with ISO Guide 31:2000.

FLX‐0119‐02‐COA Page 1 / 5

Tel 49(0)2821 48011‐10/ Fax 49(0)2821 48011‐99, e‐mail: [email protected], web: www.fluxana.com, FLUXANA® GmbH & Co.KG, Borschelstr.3, 47551 Bedburg‐Hau Germany, GM Dr. R. Schramm, reg.in Kleve HRA 2935, personal liability FLUXANA Verwaltungs‐GmbH Bedburg‐Hau, reg.in Kleve HRB 8211, FLUXANA®registered trademark



Mass fraction in % Certified value1) Uncertainty2) Traceable to Al2O3 7.36 0.10 NIST 1881A CaO 53.78 0.19 SI unit kg/kg Cr2O3 0.008 0.002 NIST 1881A Fe2O3 3.04 0.14 NIST 1881AK2O 1.23 0.03 NIST 1881A MgO 1.34 0.09 NIST 1881A Mn2O3 0.040 0.005 NIST 1881A Na2O 0.292 0.074 NIST 1881A P2O5 0.153 0.007 NIST 1881A SiO2 24.04 0.12 SI unit kg/kg SO3 total 2.43 0.05 not certified, info only SO42‐ as SO3 2.38 0.15 SI unit kg/kg SrO 0.158 0.067 NIST 1881A TiO2 0.347 0.006 NIST 1881A ZnO 0.040 0.003 NIST 1881A LOI3) 6,42 ‐ not certified, info only S2‐ 0.029 0.166 not certified, info only 1) Certified value traceable to cement NIST 1881A or SI unit kg/kg based on original sample material. 2) Expanded uncertainty UCRM calculated for a confidence interval of 95% (k=2) based on a combined

uncertainty of characterization, homogeneity and long term stability. 3) LOI is informal only and is excluded from certification because it might change over time.

The sum of all oxides is 99.99%. This includes SO3 total and LOI and excludes SO42‐ as SO3 and S2‐. Bedburg‐Hau, 26.07.2019 Responsible Reference Materials General Manager Susan Aschenbrenner Dr. Rainer Schramm

FLX‐0119‐02‐COA Page 2 / 5


Description of the CRM This reference material is an industrial product and was taken directly from the production stream. The complete batch was sealed into 30g bottles. This material is normally used as cement for constructions. Intended use Calibration and control sample for x‐ray fluorescence (XRF) analysis. Instructions for the correct use of the CRM This material is moisture sensitive. The Material has to be dried prior to use. After opening the material has to be sealed again as soon as possible to avoid any change. Otherwise it has to be ignited for minimum 1 hour at 950°C prior to use. The ignition process must result in a constant weight. The ignited material must be stored in a desiccator not longer than 24h, then reignition might be necessary. The minimum sample quantity for analysis should be 1.0g to be in agreement with the stated uncertainties. For XRF use, ignited samples should be prepared as a fused bead, e.g. in accordance with ISO 29581‐2:2010. If the sample is used after ignition 950°C to constant mass , the ignited certified values have to be calculated, using the following formula: 𝑐𝑜𝑛𝑐 𝑐𝑜𝑛𝑐 ∗ 𝑆𝑢𝑚𝑆𝑢𝑚 𝐿𝑂𝐼 The following table contains an example of certified values concoriginal recalculated to ignited sample values concignited (LOI=5,73%) as obtained directly from, e.g., a fused bead. FLX‐CRM 119 Certified values for ignited sample mass% concignited UCRM Traceable to Al2O3 7.81 0.11 NIST 1881A CaO 57.05 0.20 SI unit kg/kg Cr2O3 0.009 0.003 NIST 1881A Fe2O3 3.22 0.15 NIST 1881A K2O 1.30 0.03 NIST 1881A MgO 1.42 0.09 NIST 1881A Mn2O3 0.043 0.005 NIST 1881A Na2O 0.310 0.078 NIST 1881A P2O5 0.162 0.008 NIST 1881A SiO2 25.50 0.12 SI unit kg/kg SO3 total 2.58 0.05 not certified, info only SO42‐ as SO3 SrO 0.167 0.071 NIST 1881A TiO2 0.368 0.006 NIST 1881A ZnO 0.043 0.004 NIST 1881A LOI S2‐

FLX‐0119‐02‐COA Page 3 / 5


Expiration of Certification This certificate is valid, within the uncertainty specified, until 31.05.2025, provided the CRM is handled in accordance with instructions given in this certificate. The certification is nullified if the CRM is damaged, contaminated, or otherwise modified. Hazardous situation For this material an actual MSDS is available. Level of homogeneity In accordance with ISO Guide 35: 2006 a homogeneity study was performed. A one‐way ANOVA was used to calculate the batch inhomogeneity 𝑢 .




𝑈 𝑘 𝑢 𝑢 𝑢 Traceability The analytical work performed to assess this material was carried out by the FLUXANA laboratory, which works under DIN EN ISO/IEC 17025 accreditation. All of the results derived as part of this testing program have traceability to NIST 1881A from NIST and some additionally to the SI unit kg.

FLX‐0119‐02‐COA Page 4 / 5


Methods used In accordance with ISO Guide 34, we use the approach “measurement by a single (primary) method in a single laboratory”. An example for this approach is also found in DIN ISO 13528:2009‐01 chapter 5.4. Using this approach, samples of the test material that is to be the new reference material are prepared first. They are tested along with CRMs or synthetic RMs using a suitable method. The assigned values XCRM and their uncertainties UCRM are then derived from a calibration against the certified reference values of the CRMs. The error of the calibration used can be neglected because only the differences in the results between the new reference material and the CRM or synthetic RM are part of the evaluation. CRM used: NIST 1881A Synthetic RMs made from pure chemicals by weighing Measurement method used: ISO 29581‐2:2010‐03 Further information The following table lists all results obtained for this sample material. Values in bold represent the results with the smallest uncertainty; i.e., those used for the certification. Users who need all values traceable to a NIST CRM are provided with all results in the following table. However in comparison with the values traceable to the SI unit, they show a higher uncertainty. For comparison with the certified values, the results of an independently performed proficiency test are also given. A detailed report is available at www.fluxana.com.

FLX‐0119‐02‐COA Page 5 / 5


FLX‐CRM 119 Traceable to Traceable to For Comparison NIST 1881A SI unit kg/kg results of PT mass% XCRM UCRM XCRM UCRM XPT UPT Al2O3 7.36 0.10 7.38 0.08 CaO 53.79 0.39 53.78 0.19 54.14 0.26 Cr2O3 0.008 0.002 0.010 0.002Fe2O3 3.04 0.14 3.11 0.04 K2O 1.23 0.03 1.21 0.03 MgO 1.34 0.09 1.33 0.03 Mn2O3 0.040 0.005 0.038 0.004Na2O 0.292 0.074 0.269 0.027P2O5 0.153 0.007 0.152 0.003SiO2 23.97 0.19 24.04 0.12 23.96 0.15 SO3 total 2.43 0.05 SO42‐ as SO3 2.451) 0.15 2.38 0.153) 2.39 0.08SrO 0.158 0.067 0.155 0.008TiO2 0.347 0.006 0.352 0.006ZnO 0.040 0.003 0.039 0.003LOI 5.842) 0.12 5.73 0.123) 5.65 0.07 S2‐ 0.029 0.166

Sum (w/o SO42‐+S2‐) 100.231) Traceable to NIST 1880B. 2) Traceable to NIST 1888B. 3) UCRM taken from calculations based on NIST CRM. This certificate is in conformance with ISO Guide 31:2000.



FLUXANA


FLX-CRM 120 Cement



Cr2O3 0.005 0.002 NIST 1881A

Fe2O3 1.11 0.11 NIST 1881A

K2O 0.692 0.032 NIST 1881A

MgO 3.55 0.09 NIST 1881A

Mn2O3 0.188 0.003 NIST 1881A

Na2O 0.184 0.062 NIST 1881A

P2O5 0.086 0.006 NIST 1881A




SrO 0.124 0.337 NIST 1881A

TiO2 0.598 0.004 NIST 1881A

ZnO 0.008 0.003 NIST 1881A




uncertainty of characterization, homogeneity and long term stability. The sum of all oxides is 100.39%. This includes SO3 total and LOI and excludes SO42- as SO3 and S2-. Bedburg-Hau, 01.06.2015 Responsible Reference Materials Statistics and Report Dr. Barbara Schäfer Dr. Rainer Schramm









Al2O3 7.77 0.10 NIST 1881A


Cr2O3 0.005 0.002 NIST 1881A

Fe2O3 1.13 0.11 NIST 1881A

K2O 0.704 0.032 NIST 1881A

MgO 3.62 0.09 NIST 1881A

Mn2O3 0.191 0.003 NIST 1881A

Na2O 0.188 0.063 NIST 1881A

P2O5 0.087 0.006 NIST 1881A


SO3 total

SO42- as SO3

SrO 0.126 0.343 NIST 1881A

TiO2 0.609 0.004 NIST 1881A

ZnO 0.008 0.003 NIST 1881A

LOI

S2-






𝑛














Al2O3 7.64 0.10 7.60 0.09

CaO 53.68 0.35 53.63 0.07 53.44 0.28

Cr2O3 0.005 0.002 0.007 0.002

Fe2O3 1.11 0.11 1.20 0.02

K2O 0.692 0.032 0.656 0.023

MgO 3.55 0.09 3.51 0.04

Mn2O3 0.188 0.003 0.182 0.007

Na2O 0.184 0.062 0.194 0.026

P2O5 0.086 0.006 0.086 0.004

SiO2 26.58 0.16 26.51 0.08 26.34 0.19

SO3 total 4.35 0.14

SO42- as SO3 3.251) 0.191 3.18 0.193) 3.21 0.12

SrO 0.124 0.337 0.121 0.006

TiO2 0.598 0.004 0.597 0.011

ZnO 0.008 0.003 0.009 0.002

LOI 1.822) 0.22 1.71 0.223) 1.84 0.10

S2- 0.632 0.149

Sum (w/o SO42-+S2-) 100.13







Mass fraction in % Certified value1) Uncertainty2) Traceable to Al2O3 8.78 0.10 NIST 1881A CaO 44.45 0.05 SI unit kg/kg Cr2O3 0.008 0.003 NIST 1881A Fe2O3 3.04 0.37 NIST 1881AK2O 2.73 0.26 NIST 1881A MgO 1.41 0.09 NIST 1881A Mn2O3 0.111 0.004 NIST 1881A Na2O3) 1.23 0.15 NIST 1885A P2O5 0.112 0.006 NIST 1881A SiO2 30.81 0.10 SI unit kg/kg SO3 total 2.55 0.09 NIST 1881A SO42‐ as SO3 2.37 0.10 SI unit kg/kg SrO 0.140 0.051 NIST 1881A TiO2 0.344 0.009 NIST 1881A ZnO 0.031 0.003 NIST 1881A LOI3) 4.24 0.21 not certified, info only S2‐ 0.025 0.049 not certified, info only 1) Certified value traceable to cement NIST 1881A, NIST 1885A or SI unit kg/kg based on original sample

material. 2) Expanded uncertainty UCRM calculated for a confidence interval of 95% (k=2) based on a combined

uncertainty of characterization, homogeneity and long term stability. 3) LOI is informal only and is excluded from certification because it might change over time. The sum of all oxides is 99.97%. This includes SO3 total and LOI and excludes SO42‐ as SO3 and S2‐. Bedburg‐Hau, 26.07.2019 Responsible Reference Materials General Manager Susan Aschenbrenner Dr. Rainer Schramm



Description of the CRM This reference material is an industrial product and was taken directly from the production stream. The complete batch was sealed into 30g bottles. This material is normally used as cement for constructions. Intended use Calibration and control sample for x‐ray fluorescence (XRF) analysis. Instructions for the correct use of the CRM This material is moisture sensitive The Material has to be dried prior to use. After opening the material has to be sealed again as soon as possible to avoid any change. Otherwise it has to be ignited for minimum 1 hour at 950°C prior to use. The ignition process must result in a constant weight. The ignited material must be stored in a desiccator not longer than 24h, then reignition might be necessary. The minimum sample quantity for analysis should be 1.0g to be in agreement with the stated uncertainties. For XRF use, ignited samples should be prepared as a fused bead, e.g. in accordance with ISO 29581‐2:2010. If the sample is used after ignition 950°C to constant mass , the ignited certified values have to be calculated, using the following formula: 𝑐𝑜𝑛𝑐 𝑐𝑜𝑛𝑐 ∗ 𝑆𝑢𝑚𝑆𝑢𝑚 𝐿𝑂𝐼 The following table contains an example of certified values concoriginal recalculated to ignited sample values concignited (LOI=4,24%) as obtained directly from, e.g., a fused bead. FLX‐CRM 121 Certified values for ignited sample mass% concignited UCRM Traceable to Al2O3 9.17 0.10 NIST 1881A CaO 46.42 0.05 SI unit kg/kg Cr2O3 0.008 0.003 NIST 1881A Fe2O3 3.17 0.39 NIST 1881A K2O 2.85 0.28 NIST 1881A MgO 1.47 0.09 NIST 1881A Mn2O3 0.116 0.004 NIST 1881A Na2O 1.28 0.15 NIST 1885A P2O5 0.117 0.007 NIST 1881A SiO2 32.18 0.10 SI unit kg/kg SO3 total 2.66 0.09 NIST 1881A SO42‐ as SO3 SrO 0.146 0.053 NIST 1881A TiO2 0.360 0.009 NIST 1881A ZnO 0.033 0.003 NIST 1881A



LOI S2‐ Expiration of Certification This certificate is valid, within the uncertainty specified, until 31.05.2025, provided the CRM is handled in accordance with instructions given in this certificate. The certification is nullified if the CRM is damaged, contaminated, or otherwise modified. Hazardous situation For this material an actual MSDS is available. Level of homogeneity In accordance with ISO Guide 35: 2006 a homogeneity study was performed. A one‐way ANOVA was used to calculate the batch inhomogeneity 𝑢 .




𝑈 𝑘 𝑢 𝑢 𝑢 Traceability The analytical work performed to assess this material was carried out by the FLUXANA laboratory, which works under DIN EN ISO/IEC 17025 accreditation.



All of the results derived as part of this testing program have traceability to NIST 1881A from NIST and some additionally to the SI unit kg. Methods used In accordance with ISO Guide 34, we use the approach “measurement by a single (primary) method in a single laboratory”. An example for this approach is also found in DIN ISO 13528:2009‐01 chapter 5.4. Using this approach, samples of the test material that is to be the new reference material are prepared first. They are tested along with CRMs or synthetic RMs using a suitable method. The assigned values XCRM and their uncertainties UCRM are then derived from a calibration against the certified reference values of the CRMs. The error of the calibration used can be neglected because only the differences in the results between the new reference material and the CRM or synthetic RM are part of the evaluation. CRM used: NIST 1881A Synthetic RMs made from pure chemicals by weighing Measurement method used: ISO 29581‐2:2010‐03 Further information The following table lists all results obtained for this sample material. Values in bold represent the results with the smallest uncert

CERTIFICATE OF ANALYSIS FLX-CRM 113 Cement...2 O 3 5.14 0.07 NIST 1880B CaO 64.61 0.25 SI unit kg/kg...

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Transcript of CERTIFICATE OF ANALYSIS FLX-CRM 113 Cement...2 O 3 5.14 0.07 NIST 1880B CaO 64.61 0.25 SI unit kg/kg...