Certified Reference Material

Reference material certificate

Antimony Standard for ICP

Product no.: 73495

Lot no.: BCCK7468
Description of CRM: Antimony semimetal (high-purity quality) in 1.8% HNO3 and 0.05% HF
(prepared with acids suitable for trace analysis and high-purity water,
18.2 MΩ∙cm, 0.22 µm filtered).
Expiry date: AUG 2027 (unopened bottle in aluminized bag)
Storage: Store at 5°C-25°C
Density (certified) at 20°C: 1010 kg m-3 ± 1 kg m-3

Constituent Certified values at 20°C and expanded uncertainties, U = k . u (k = 2) [1][2]

Antimony 992 mg kg-1 ± 4 mg kg-1 1002 mg L-1 ± 5 mg L-1

[3]
Metrological traceability: Directly traceable to NIST SRM 3102a / ICP-OES.
Measurement method: The certified value is established by inductively coupled plasma optical emission
spectrometry ICP-OES in accordance with ISO/IEC 17025.[4]
Intended use: Calibration of ICP, AAS, spectrophotometry or any other analytical technique.
Instructions for handling The bottle’s temperature must be 20°C. Shake well before every use. If storage
and correct use: of a partially used bottle is necessary (at the user`s risk), the cap should be
tightly sealed and the bottle should be stored at reduced temperature (e.g.
refrigerator) to minimize transpiration rate.
Health and safety Please refer to the Safety Data Sheet for detailed information about the nature
information: of any hazard and appropriate precautions to be taken.
Packaging: 100 mL HDPE bottle sealed with an aluminized bag
Accreditation: Sigma-Aldrich Production GmbH is accredited by the Swiss Accreditation Service
SAS as reference material producer under no. SRMS 0001 in accordance with
international standard ISO 17034[5]
Certificate issue date: 30 NOV 2023

ISO 17034 S. Matt – CRM Operations Dr. P. Zell – Approving Officer

SRMS 0001

Sigma-Aldrich Production GmbH, Industriestrasse 25, 9471 Buchs, Switzerland;

Tel +41-81-755-2511; Fax +41-81-756-5449; www.sigmaaldrich.com
Sigma-Aldrich Production GmbH is a subsidiary of Merck KGaA, Darmstadt, Germany.

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 Certification process details:

The certified value of the content (mg/kg) is determined using high-performance inductively coupled plasma
optical emission spectrometry (HP-ICP-OES). To obtain performance comparable to isotope dilution and
classical methods (titration and gravimetric analysis) the HP-ICP-OES measurement is performed using an
internal standard and a drift correction procedure. [6]
The mean value is based on 20 measurements (two samples and 10 measurements per sample). All
measurements are traced gravimetrically to an internationally accepted reference material e.g. from NIST
(USA) or BAM (Germany).

Homogeneity assessment:
Due to the production process, a homogeneous solution derives. Nevertheless a small homogeneity contribution
is included into the calculation of content uncertainty of this CRM.

Stability assessment:
The storage behavior of standard solutions is of greatest importance with regard to the certified value. Therefore
the two most important effects were investigated by in-depth studies in a cooperation with EMPA, St. Gallen:
1. The leachate from HDPE (high- Transpiration through 100 mL HD-PE bottles
density polyethylene) bottles was
analyzed by HR-ICP-MS after leaching 1.008
the bottles with 2 % nitric acid. measured (mean of 9 bottles)
Maximum contamination levels were extrapolated 30°C
Increase of concentration

found in the ng L-1 level for 12

relative to 1.000 gL-1

1.006
elements. Bottle stored
2. To avoid significant loss of mass without Al-bag

through transpiration the bottle is

1.004
delivered in aluminum coated bags.
23°C
After the bottle has been removed
from the bag, transpiration will occur
at an accelerated rate (see figure). We 1.002
highly recommend not opening the Bottle stored
in Al-bag, 23°C
bag until the solution is needed. Once
the bottle is opened the solution 1.000
should be stored at reduced 0 360 720 1080
1 2 3
temperature (4 °C) to reduce Years
transpiration.

Density Measurement:
The density measurement is carried out in accordance with ISO/IEC 17025[4] using an in-house method.

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 Uncertainty evaluation:
The uncertainty contributions are illustrated by the following cause-effect diagram:
Typical relative contributions are:
u(wCRM) 0.1 – 0.3 % Determination Determination
uhom < 0.03 % of Content of Density
ustab < 0.09 % (wCRM) ()
u(ρ) < 0.05 % Reference

Repeatability
Certified
Value of CRM
Homogeneit Bottle leaching

Solvent quality Transpiration

Homogeneity Stability
(hom) (stab)

The combined standard uncertainty is calculated by combination of the standard uncertainties of the input
estimates according to Eurachem/CITAC Guide “Quantifying Uncertainty in Analytical Measurement” and
ISO 17034.[2][5]

Expanded uncertainty is then calculated to a confidence level of 95%, typically by multiplying with a confidence
level factor of k=2.

Trace Impurities:
Up to 75 trace impurities were analyzed by ICP-OES, ICP-MS and AAS. Some of the impurities are determined
in the starting material and calculated for the solution (e.g. for rare earth elements contamination during the
preparation is rendered impossible). Other elements are determined both in the starting material as well as in
the bottled solution.
All values listed below are given in mg kg-1 (ppm), <X = below detection limit, m = matrix, n.a. = not analyzed

Li Be B C N O F Ne
<0.010 <0.005 <0.010 n.a. n.a. n.a. n.a. n.a.
Na Mg Al Si P S Cl Ar
<0.025 <0.005 <0.025 n.a. n.a. n.a. n.a. n.a.
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
<0.050 <0.010 <0.002 <0.005 <0.010 <0.010 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010 <0.001 <0.025 <0.001 <0.002 n.a. n.a.
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
<0.001 <0.005 <0.001 <0.010 <0.001 <0.010 n.a. <0.001 <0.001 <0.001 <0.020 <0.010 <0.001 <0.025 m <0.001 n.a. n.a.
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
<0.001 <0.005 0.067 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.050 <0.050 <0.025 n.a. n.a. n.a.
Fr Ra Ac
n.a. n.a. n.a. Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
<0.001 <0.001 <0.001 n.a. <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001 <0.001
Th Pa U
<0.001 n.a. <0.001

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 References:
[1] ISO Guide 35:2017, “Reference materials - Guidance for characterization and assessment of
homogeneity and stability”
[2] Eurachem/CITAC Guide, 3 rd Ed. (2012), “Quantifying uncertainty in analytical measurement”
[3] Eurachem/CITAC Guide, 2 nd Ed. (2019), “Metrological Traceability in chemical measurement”
[4] The accredited testing laboratory STS 0490 performs the measurements and weighing steps for the
certification of this CRM under ISO/IEC 17025:2017, “General requirements for the competence of
testing and calibration laboratories”
[5] ISO 17034:2016, “General requirements for the competence of reference material producers”
[6] Marc L. Salit et al., Anal. Chem. 2001, 73, 4821-4829, “Single-Element Solution Comparisons with a
High-Performance Inductively Coupled Plasma Optical Emission Spectrometric Method”

Certificate of analysis revision history:

Certificate version Certificate issue date Reason for version

01 30 NOV 2023 Initial version

Disclaimer:
The purchaser must determine the suitability of this product for its particular use. Sigma-Aldrich Production
GmbH makes no warranty of any kind, express or implied, other than its products meet all quality control
standards set by Sigma-Aldrich Production GmbH. We do not guarantee that the product can be used for a
special application.

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© 2018 Merck KGaA, Darmstadt, Germany and/or its affiliates. All Rights Reserved.

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