ELEMENTAL

TRACE ANALYSIS
Certified Reference Materials and High Purity
Reagents for Elemental Analysis

Zuzana Antalov
May 16, 2017
Cluj, Romania
Inorganic Trace Analysis
High-purity reagents and standards
manufactured to clear, guaranteed specifications

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CALIBRATION
Certified Reference Materials
TraceCERT

TraceCERT CRMs are high accuracy standards for instrument calibration and process
validation

Atomic Spectroscopy CRMs TraceCERT

Multi-Element Standards for ICP
Single-Element Standards for AAS
Single-Element Standards for ICP
Custom Standard Solutions

Ion Chromatography CRMs TraceCERT

PRIMUS (Primary Multi-ion Standards)
Multi-ion Standards
Inorganic Anion Standards
Inorganic Cation Standards
Custom Standard Solution
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TRACECERT CRMS
FOR AAS AND ICP
Certified Reference Materials
TraceCERT are characterized by

Highest-purity starting materials available

Superior level of accuracy, very low uncertainties and lot-specific values
Traceability to at least two independent references (i.e. NIST, BAM or SI unit kg)
Comprehensive documentation (certification according to ISO Guide 31)
Certificates of ICP standards list up to 70 trace impurities
ICP standards packaged in light- and gas-tight aluminum foil bags (for extended stability)

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Certified Reference Materials
Certification process

Schematic representation of the

production design and certification
of TraceCERT products.

This approach was established for

the preparation of inter-comparison
samples at the highest metrological
stage.

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 Certified Reference Materials
www.sigmaaldrich.com/tracecert
Inorganics for Spectroscopy

AAS, Certified single element standard

solutions (1000mg/L) suitable for AAS,
Single element, AAS
Supplied in HDPE bottles except for Hg
(borosilicate white glass)

ICP, Certified solutions (1000mg/L) and

tested for up to 70 trace impurities,
Single element, ICP
Supplied in HDPE bottles and sealed into
an aluminium bag, including the
certificate
AAS & ICP, concentrated solutions
Single element, AAS, (10000 mg/L) also available for many
ICP elements. Sealed in an aluminium bag
and delivered with the printed certificate

Multi-element, a wide variety of mixes

based on a chemical class or periodic
Multi- element, ICP table sections, and also specific mixes for
ICH Q3D testing

Custom standard for AAS and ICP using our online custom
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solutions standards platform
 Inorganics for Spectroscopy
Multi-element mixes for ICP

Periodic Table Mixes Chemical Group Mixes

Mix 1 for ICP (33 elements), # 92091 Alkali Metals (100mg/L, #96441)

Mix 2 for ICP (17 elements), # 41135 Alkaline Earth (100mg/L, #67288)

Mix 3 for ICP (16 elements), # 78334 Rare Earth (50mg/L, #67349)
Metalloid and non-metals (100mg/L,#55263)

All components are present at a Post-transition metals (100mg/L, #51509)

concentration of 10 mg/l Transition metal mixes 1, 2, 3 (100mg/L,
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#04330, 96442, 93468)
TraceCERT
Certification and Comprehensive Documentation

A detailed and comprehensive certificate of up to four pages, in accordance with ISO Guide 31

Example:
ICP Platinum

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TraceCERT
Certification and Comprehensive Documentation

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TRACECERT CRMS
FOR IC
 Certified Reference Materials
For Ion Chromatography www.sigmaaldrich.com/tracecert

Single element Inorganic Anion Standards, 1000 mg/l

Single element Inorganic Cation Standards, 1000 mg/l

Multi element PRIMUS (Primary Multi-ion Standards),

10mg/kg each (inorganic anions, cations)

Multi-ion Standards Multi-ion Standards, various

concentration and solvents

Custom standard for IC using our online custom standards

13 solutions platform
 Certified Reference Materials
For Ion Chromatography
Primary multi-anion and cation standard
solutions
PRIMUS
Starting materials are characterised by
EMPA and BAM
Sealed in an Al bag for long term stability
Detailed printed certificate provided
Recommended by Metrohm for the calibration
and validation of their instruments

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 Inorganics for Spectroscopy
Cant find exactly what you need?

TraceCERT Custom
Standards are:
Wit High accuracy and
reliability of certified
concentrations
Traceable to NIST
standards and other
accepted references
Certified according to
ISO/ IEN 17025 and ISO
TraceCERT Custom Standard Solutions Guide 34 and supplied
with a CoA according to
ISO Guide 31
Elemental AAS, ICP Anions and Cations
Packaged specially to
for Ion Chromatography ensure maximum shelf life

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SAMPLING AND
SAMPLE
PREPARATION
HIGH PURITY
ACIDS & BASES
AND SALTS
High Purity Acids and Bases
Suprapur acids and bases | Ultrapur acids

Advantages
Choose your purity grade for instrumental trace analysis
Suprapur acids filled in borosilicate glass or extra pure HDPE material
Ultrapur acids filled in PFA bottles
Certificate of Analysis gives an extensive impurity profile

Quality grades
for your
individual needs
High Purity Acids and Bases
Different grades to meet your needs

Ultrapur acids
High purity acids, hydrogen peroxide
Highly sophisticated instrumental ultra-trace analysis, e.g. ICP-MS
Specified parameters in ppt range
Ultrapur acids are preferred for ultra-trace analysis in the pg/g (ppt)
range

Suprapur acids and bases

High purity acids and bases
Highly sophisticated instrumental trace analysis, e.g. AAS and ICP-OES
Specified parameters in ppb range
Suprapur acids and bases are suitable for trace analysis in the ng/g
(ppb) range

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High Purity Acids and Bases
Suprapur acids and bases | Ultrapur acids

Suprapur acids and bases are suitable for trace Ultrapur acids are preferred for ultra-
analysis in the ng/g (ppb) range trace analysis in the pg/g (ppt) range

Suprapur acids are filled in borosilicate or extra pure PE bottles.
The material minimizes any elemental impurity of the acid, so the
specification of the unopened bottle is kept during the minimum
shelf life. The bottles are cleaned and pre-conditioned before filling.
Quality control is done after filling. This gives you the assurance
that the certified batch values are those values of the filled acid.
Suprapur reagents are packed in a stable outer-box.
Hydrogen peroxide Suprapur is packed in a black bottle to protect
it against light. The bottle is made of extra pure PE material to avoid
any contamination. To make it more safe for you: hydrogen peroxide
bottles are closed with the SafetyCap. The SafetyCap with the PTFE
membrane releases the pressure, but avoids any contamination.
Ultrapur reagents are produced by subboiling
distillation. The slowly distilled reagents subsequently
have the lowest possible trace-impurities. Ultrapur
reagents are exclusively filled in pre-conditioned PFA
(fluorpolymer) bottles. This material meets the
highest demands of all users for ultratrace
instrumental analysis, e.g. ICP-MS. Ultrapur reagents
are packed in a stable
outer-box.

Raw material production

Filling of Quality Certificate
the bottle Control of Analysis
Packaging Conditioning of
material the bottle

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High Purity Acids and Bases
Suprapur acids and bases | Ultrapur acids in a nutshell

a high quality during the shelf life of the product

a high batch-to-batch consistency
realistic values on the Certificate of Analysis

Raw material production

Filling of Quality Certificate
the bottle Control of Analysis
Packaging Conditioning of
material the bottle

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High Purity Acids and Bases
CoA

Certificate of Analysis provides:

Assay
Extended impurity profile
Minimum shelf life

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High purity acids and bases - Suprapur
Product Range

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High purity acids and bases - Ultrapur
Product Range

High density PFA;

smooth surface

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High Purity Acids and Bases
HDPE dosage bottle for hydrofluoric acid

HDPE dosage bottle

250 and 500 mL bottle with a withdrawal system especially constructed for
this hazardous acid (Ord. No.: 1.00335.0250 and 1.00335.0500)
Allows drop-by-drop withdrawal and the last drop stays reliably in the bottle
Special density function of our exclusive S40 screwing system
Allows transportation and storage in cardboard boxes

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High Purity Acids and Bases
SafetyCap the intelligent closure

Leakproof against liquids allows excess pressure to be

released

Allows gas to be released and the internal pressure to be decreased

Allows no liquid to escape, thus protecting the environment from contamination

Hydrogen peroxide Suprapur

Ord. No.: 107298.0250, 107298.0500 and 107298.1000

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AAS Auxiliaries

Matrix modifier for GF-AAS Spectroscopic buffers for F-AAS

(graphite furnace atomic absorption spectrometry) (flame atomic absorption spectrometry)

Magnesium matrix modifier Cesium chloride-aluminum nitrate buffer solution

According to Schuhknecht and Schinkel
c(Mg)= 10.0 0.2g/l (contains 50g/l CsCl and 250g/l Al(NO3)3)
[Mg(NO3)2 in 15 % HNO3]

Palladium matrix modifier Cesium chloride-lanthanum chloride

c(Pd)= 10.0 0.2g/l Buffer solution according to Schinkel
[Pd(NO3)2 in 15 % HNO3] (contains 100g/l La and 10g/l CsCl)
Phosphate matrix modifier Cesium chloride solution
c(NH4H2PO4)=1000.2g/l c(CsCl)= 20g/l
[NH4H2PO4 in water] in water
Ammonium dihydrogen phosphate Suprapur Lanthanum (III) oxide
Suitable as matrix modifier

L-(+)-Ascorbic acid GR

Reagents for use in sample preparation as well as in calibration for

optimizing analysis conditions comprises selected matrix modifiers and
spectroscopic buffers for AAS measurements

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 High purity salts - Suprapur
Improved flowability and chemical purity

Production and Quality Control is done in Darmstadt following

modern and sophisticated methods and crystallization techniques
This ensures the high purity of the salt:
Purity 99.99% or up to 99.9999%
Extensive impurity profile of the product
on the CoA
Suitable for sample preparation
of elemental trace analysis

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Inorganic Trace Analysis
Certified Eluent Concentrates for IC

The certified eluent concentrates for ion chromatography are traceable by potentiometric titration to NIST
Standard Reference Materials and certified in accordance with ISO Guide 31. All details about exact
content, uncertainty, traceability and expiry date are described in the certificate.

Single Concentrates
Binary Concentrates
the selection of well-characterized eluent concentrates, a novel group of binary concentrates (20-fold
concentration)
The key features are
1. Application tested using Metrohms Metrosep columns
2. Certificate according to ISO Guide 31
3. High-purity starting materials
4. All details about the exact content, specifications, and expiry date are described in the certificate
5. Packaging: 1 L and 2.5 L HDPE bottles with 45 mm screw thread

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Inorganic Trace Analysis
Water for IC

A water quality especially for the needs of ion chromatography

This water is also suitable for trace analysis of anions, cations and also some organics which are usually
analyzed by IC
The product is delivered in HDPE bottles with 45 mm thread

Specification
Organic traces 10 g/kg each: acetate, formiate, glycolate, oxalate
Cation traces
5 g/kg each: Al, Ba, Bi, Cd, Co, Cr, Cu, Fe, Li, Mg, Mn, Mo, Ni, Pb, Sr, Zn
10g/kg each: Ca, K, Na, NH4+
1 g/kg each: bromide, bromate, chlorate, chloride, chlorite, fluoride, iodide, nitrate, nitrite,
Anion traces
phosphate, sulfate
Conductivity 2 S/cm

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METHOD DEVELOPMENT
AND VALIDATION
Inorganic Trace Analysis
Matrix CRMs from the European Commissions Joint Research Centre

CRMs with Certified Elemental Content

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Inorganic Trace Analysis
Qualification Kit for IC
The kit is intended for testing detection linearity, injector precision and injector carry-over

The 50 mg/kg standard is used for repeatability tests (injector precision) and the maximum
carry-over during injection is verified with the 1000 mg/kg standard.
The standards 5 to 100 mg/kg are used to prove the detector linearity

It is a special advantage that the certified bromide standards (produced in a double

accredited laboratory fulfilling ISO/IEC 17025 and ISO Guide 34) can be used for
conductivity, UV/Vis and electrochemical detectors

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Inorganic Trace Analysis
Proficiency Testing Process and Products

Proficiency testing products accredited by ACLASS to ISO/IEC 17043:2010

Certificate No. AP-1469 and recognized by accreditation bodies worldwide
Application
fields
1. Registration & order
Prior to your first order, you must obtain a lab code by registering on the PT portal.
2. Delivery
Participating labs receive blind samples according to schedule.
3. Open study
Each lab analyzes the blind samples.
4. Reporting
Labs report results on the PT portal before the study closes.
5. Data processing
Data is processed to issue individual evaluation reports.
6. Evaluation report
Reports are sent via the PT portal. If requested, a copy is sent to your accreditation body.
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THANK YOU.