2.

Titration – Volumetric Reference Materials

Accurate titer determination is an important criterion for precise and comparable
titration analysis. Our offering of Certipur® volumetric standards include high-
purity secondary reference materials for acidimetry, alkalimetry, argentometry,
complexometric, iodometry and redox titration.

Features & Benefits

• Highly pure materials traceable to NIST

• In accordance with the reagents part of major Pharmacopoeias

• Measured in ISO 17025 accredited laboratory

• Branded as CRMs in accordance with ISO 17034

Table 2. Volumetric Standards

Product Product
Product Name Applications Product Name Applications
Number Number
Potassium hydrogen phthalate, Calcium carbonate, volumetric
Volumetric standard, secondary standard, secondary reference
reference material for alkalimetry, material for complexometry,
1.02400 1.02410
traceable to NIST Standard traceable to NIST, Standard
Reference Material (SRM), Certipur® Reference Material (SRM), Certipur®
Reag. Ph. Eur., Reag. USP1,2 Reag. USP2 Complexometry
Alkalimetry
Benzoic acid, volumetric standard, Zinc, volumetric standard,
secondary reference material for secondary reference material for
1.02409
alkalimetry, traceable to NIST, complexometry, traceable to NIST,
1.02401
Standard Reference Material (SRM), SRM Certipur® Reag. Ph. Eur.1
Certipur® Reag. Ph. Eur., Reag.
Potassium iodate, volumetric
USP1,2
standard, secondary reference
1.02404 Iodometry
Sodium carbonate, volumetric material for iodometry, traceable to
standard, secondary reference NIST SRM, Certipur®
1.02405
material for acidimetry, traceable to
Glycine, analytical standard, for
NIST SRM, Certipur®1
94119 Nitrogen Determination according to
Tris(hydroxymethyl)aminomethane, Acidimetry Kjeldahl Method3
volumetric standard, secondary Kjeldahl Method
Kjeldahl Nitrogen, Total (TKN) 1000
reference material for acidimetry,
1.02408 TKN1000 mg/L Calibration Standard, certified
traceable to NIST, Standard
reference material3
Reference Material (SRM), Certipur®
Reag. Ph. Eur., Reag. USP2
1
Solution according to Reag. Ph. Eur
Sodium chloride, volumetric 2
Solution according to the reagents chapter of USP
standard, secondary reference
1.02406 material for argentometry, traceable Argentometry 3
BAM Certification
to NIST SRM, Certipur® Reag. Ph.
Eur. ,Reag. USP1,2
Explore our Volumetric Reference Materials
di-Sodium oxalate, volumetric
standard, secondary reference Our broad portfolio of volumetric reference materials is
1.02407 material for redox titration, traceable available in different concentrations and packaging.
to NIST, Standard Reference Material
(SRM), Certipur® Reag. USP2 Please find more information on our Titripur®
Iron (II) ethylenediammonium Volumetric Solutions, Titripac® Packaging for
sulfate, Volumetric standard, Volumetric Solutions, Titrisol® Volumetric Concentrates,
secondary reference material for Redox Titration SmartChemicals for Digitalized Titration & 3S Reagents
1.02402
redox titration, traceable to NIST,
Standard Reference Material (SRM), for Digitalized Volumetric Titration by clicking the link:
Certipur® Reag. Ph. Eur.1
SigmaAldrich.com/titration-reagents
Potassium dichromate, volumetric
1.02403
standard, secondary reference Find detailed information about these products in the
material for redox titration, traceable Volumetric Titration Brochure: Volumetric Solutions and
to NIST, SRM Certipur® Reag. USP2
Standards for Titration

10
 www.sigmaaldrich.com

Certification Report – Certified Reference Material

Certipur® Volumetric Standards

Manufacturer: Merck KGaA, Frankfurter Str. 250, 64293 Darmstadt,

Germany, Tel. +49(0)6151 720
Accreditation:

Merck KGaA, Darmstadt, Germany is accredited by the

German accreditation authority as registered reference
material producer (D-RM-15185-01-00) in accordance with
ISO 17034.
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Introduction:
This certification report contains additional information about certified values and uncertainties, homogeneity,
stability, traceability and other relevant details of Certipur® Volumetric standards.

The scope of the ISO 17034 accreditation is documented in the annex to the accreditation certificate D-RM-
15185-01-00. The Volumetric standards are produced, characterized and certified by the legal entity Merck KGaA,
Darmstadt, Germany.

Preparation and packaging of CRMs:

Certipur® Volumetric standards are prepared from high purity salts. The mass fraction is measured by means of
potentiometric titration.

Certipur® Volumetric standards are delivered in glas bottles. The label on the products is in accordance to ISO
Guide 31 and covers ordering number, article description, lot number, expiry date and safety data information.
Packaging material is subject to comprehensive stability studies according to ISO Guide 35.

Homogeneity:
Homogeneity studies were conducted in accordance with ISO Guide 35.

A representative number of samples packaged in their final form was chosen systematically (stratified over the
whole batch) for assessment of the between-unit homogeneity. Measurements have been carried out according to
DIN EN ISO/IEC 17025. Results from multiple samples of the chosen bottles were evaluated.

Typical homogeneity contributions to uncertainty uhom are in the range of 0.03%.

An evaluation of within-bottle (within-unit) homogeneity was conducted for assessment of the minimum sample
size and does therefore not contribute to the uncertainty budget of this certified reference material. The minimum
weigh-in quantity depends on the volumetric standard and is mentioned on the certificate of analysis.

Stability:
Stability studies were conducted in accordance to ISO Guide 35.

Stability comprises long- term stability, which is associated with the storage behavior of the CRMs under
recommended storage conditions as well as short-term (transportation) stability that takes any extra effects due to
transport of the products into account (quantification of transport effects that result from temperature variations
during shipment).

Merck KGaA, 64271 Darmstadt, Germany, Tel. +49(0)6151 72-2440

EMD Millipore Corporation, 400 Summit Drive, Burlington MA 01803, USA, Tel. +1-978-715-4321
Sigma-Aldrich Canada Co. or Millipore (Canada) Ltd. 2149 Winston Park, Dr. Oakville,
Ontario, L6H 6J8, Phone: +1 800-565-1400

Certification report version 01

 Long-term stability:
Long-term stability of the products was evaluated using the classical experimental layout. Samples were stored at
the recommended storage conditions before measurement. Measurements were conducted according to DIN EN
ISO/IEC 17025. Results were evaluated using linear regression and ANOVA and the calculated uncertainty included
into the uncertainty budget as long-term stability contribution ults.

Typical long-term stability contributions to uncertainty ults are in the range of 0.02%.

Short-term (transportation) stability:

Short-term (transportation) stability was evaluated using the classical experimental layout. Samples were stored
at elevated temperatures that may arise during shipment of the products before measurement. Results were
evaluated using linear regression and ANOVA and the calculated uncertainty included into the uncertainty budget
as short- term (transportation) stability contribution usts .

Typical short-term (transportation) stability contributions to uncertainty usts are in the range of 0.01%.

Stability monitoring:
Merck KGaA, Darmstadt, Germany will monitor all Certipur® Volumetric standards over the period of their
certification (until expiry date). If substantive technical changes occur that affect the validity of certification, the
customer will be notified.

Characterisation:
Characterisation of Certipur® Volumetric standards is carried out by the accredited quality control (QC) laboratory
at Merck KGaA, Darmstadt, Germany according to DIN EN ISO / IEC 17025 by measuring the mass fraction by
potentiometric titration. Typical characterisation contributions to uncertainty uchar are in the range of 0.010 –
0.025% depending on the volumetric standard.

Traceability:
All certified values of Certipur® Volumetric standards are directly traceable to the corresponding / suitable primary
standard from NIST (NIST: National Institute of Standards and Technology).

Uncertainty evaluation:
The expanded uncertainty UCRM reported with the certified values is calculated in accordance to GUM and EA-4/02,
with k=2 as the coverage factor for a 95% coverage probability. Uncertainty contributions to the certified
expanded uncertainty are illustrated by the following cause-and-effect-diagram (Ishikawa-Diagram):

uhom ults

Homogeneity Storage
uCRM

Transport Characterisation

usts uchar

Merck KGaA, 64271 Darmstadt, Germany, Tel. +49(0)6151 72-2440

EMD Millipore Corporation, 400 Summit Drive, Burlington MA 01803, USA, Tel. +1-978-715-4321
Sigma-Aldrich Canada Co. or Millipore (Canada) Ltd. 2149 Winston Park, Dr. Oakville,
Ontario, L6H 6J8, Phone: +1 800-565-1400

Certification report version 01

 The expanded uncertainty uCRM is obtained from the standard uncertainties of characterisation, homogeneity and
stability:
UCRM = k · uCRM

uCRM = √ u2Characterisation + u2Homogeneity + u2Stability

u2Stability = u2sts + u2lts

Quality management system:

Certipur® Volumetric standards have been prepared and certified under an ISO 9001 quality management
system in accordance to
ISO 17034: General requirements for the competence of reference material producers
ISO Guide 35: Reference materials – Guidance for characterization and assessment of homogeneity and stability
ISO Guide 31: Reference materials – Contents of certificates, labels and accompanying documentation
Eurachem / CITAC Guide: Quantifying uncertainty in analytical measurement Guide to the Expression of
Uncertainty in measurement (GUM)
DIN EN ISO / IEC 17025: General requirements for the competence of testing and calibration laboratories

The vibrant M, Supelco, Certipur and Sigma-Aldrich are trademarks of Merck KGaA, Darmstadt, Germany or its
affiliates.
Detailed information on trademarks is available via publicly accessible resources.
© 2023 Merck KGaA, Darmstadt, Germany and/or its affiliates. All Rights Reserved.

The life science business of Merck KGaA, Darmstadt, Germany operates

as MilliporeSigma in the U.S. and Canada.

Certification report version 01