Ion Chromatography

PRIMUS (Primary Multiions Standards for Ion Chromatography) - A Corporate Project of:

The need of using CRM's

Today, Ion Chromatography (IC) is an important technique within the analytical laboratory. It is used for the aqueous determination of ions down to the ppt range, being one of the best methods that can provide quantitative analysis of ions at this level. Moreover, the development of modern IC apparatus and columns makes this technique a fast, uncomplicated and reliable tool.

The quality of IC standards had to be improved to keep up with the advances in the available hardware. The selection of appropriate standards for the calibration of the IC system is important. Fluka already offers a wide range of IC standards, starting from single elements for anion and cation analytic to multielement standards. These standards are frequently used by the Environmental, Food and Beverage industries. However, other industries like Pharmaceutical or Semiconductor, may need to work with even higher qualifications and certified standards to comply with GMP. This trend is furthermore reinforced by official regulations of the European Community within the guideline 96/23/EG on the use of Certified Reference Materials (CRM):
...In paragraph 3.1.1.2., the determination of trueness (one component of accuracy) is described: trueness can only be established by means of CRM's. A CRM should be used whenever available] (1).
The American FDA (Food and Drug Administration) demands in their Inspection Guide for analytic methods the usage of reference standards.

ISO (International Organization for Standardization) has published more then 6 papers about reference materials.
CRM's are guaranteed as validation standards. This means that they have to be traceable to a SI unit and standard deviation has to be determined. In accordance to ISO Guide 17025 (2), the preparation of a CRM ideally is carried out by metrological institutes such as NIST (National Institute of Standards and Technology), EMPA (Swiss Federal Laboratories for Materials Testing and Research) or BAM in Germany (Federal Institute for Materials Research and Testing).

Single- and Multielement Standards developed in collaboration with EMPA and BAM

For Ion Chromatography, the number of CRM's available is still small. In order to fill this gap, Fluka launched a few months ago their first multiion CRM's for Ion Chromatography (Table 1).
The development was carried out in collaboration with EMPA, located in St. Gallen, Switzerland. Based on the competence of this highly regarded metrological institute, the traceability to SI is guaranteed and standard deviation is determined. Therefore, these CRM's are produced completely at EMPA, giving you the guarantee of certification you desire.

Following a positive customer response, we were also asked to produce certified multielement standards and we are pleased to offer two new certified multielement standard solutions, PRIMUS (Primary Multiion Standards) (Table 2).

High precision weighing and high purity salts for highest quality

EMPA determines the purity of the starting materials based on high purity salts (Table 2). The content of these primary materials is determined by two methods for each salt. The analysis is done in collaboration with BAM. The results are verified and cross-checked at state-of-the-art levels to ensure the quality you require. The really novel part is the production procedure. First, the solid salts are determined and then they are dissolved in high purity water. Although it sounds simple, one of the core competences of EMPA is the extremely precise and accurate weighing of these salts. This allows us to offer our customers CRM's standards having a very low content of ion species (10mg/kg for each ion). To ensure the quality of our products, each bottle is delivered in a sealed aluminium bag to minimise the loss of water and to keep the concentration stable over more than two years. All standards are delivered with a Certificate of Analysis, including a detailed report with the calculation of the measurement uncertainty.

Did you know that ...

... each new Metrohm IC apparatus contains a pack of our PRIMUS multication and
multianion standards?

References

1. Commission decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Official Journal of the European Communities, L 221/8
2. ISO Guides 30 (1992): Terms and definitions used in connection with reference materials; 31(2000): Reference materials - contents of certificates and labels; 32 (1997): Calibration in analytical chemistry and use of certified reference materials; 33 (2000): Uses of certified reference materials; 34 (2000): General requirements for the competence of reference material producers; 35 (1989): Certification of reference materials - General statistical principles

www.sigma-aldrich.com/certified_standards

Table 1: PRIMUS: Multielement Standard Solutions for Ion Chromatography (10 mg/kg)

Catalog No.	Product Name	Ions	Produced from	Example Certificate
89316	Certified Multication Standard Solution	Lithium, Sodium, Potassium, Magnesium, Calcium	Li2CO3, NaCl, KCl, MgO, CaCO3
89886	Certified Multianion Standard Solution	Fluoride, Chloride, Bromide, Nitrate, Phosphate, Sulfate	NaF, NaCl, NaBr, NaNO3, Na2SO4, Na2HPO4
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PRIMUS standards supplied in 50 mL HDPE bottles. A detailed certificate is provided with each bottle including: SI traceable content, uncertainty, trace impurities and expiry date.

Catalog No.	Product Name	Produced from	Example Certificate
87969	Bromide	NaBr
87603	Chloride	NaCl
80373	Fluoride	NaF
86576	Nitrate	NaNO3
81193	Phosphate	Na2HPO4
80218	Sulfate	Na2SO4
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These certified standards are prepared with high-purity salts and water and are supplied in 100 mL HDPE bottles.

click here for Background Information

Cat. No.	Ion	Composition	Example Certificate	Additional Information
59755	Ammonium	NH4Cl in water		replaces cat. no. 95023
43147	Bromide	NaBr in water		replaces cat. no. 17355
39883	Chloride	NaCI in water		replaces cat. no. 24889
40121	Chromate	KCrO4 in water		replaces cat. no. 27072
90157	Cyanide
77365	Fluoride	NaF in water		replaces cat. no. 47070
41271	Iodide	KI in water		new product
74246	Nitrate	NaNO3 in water		replaces cat. no. 72547
67276	Nitrite	NaNO2 in water		replaces cat. no. 77012
38364	Phosphate	Na2HPO4 in water		replaces cat. no. 79409
90071	Sulfate	Na22SO4 in water		replaces cat. no. 86126
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Our new certified eluent concentrates for ion chromatography are traceable by potentiometric titration
to NIST Standard Reference Material. It is certified in accordance with ISO Guide 31. All details about
exact content, uncertainty, traceability and expiry date are described in the certificate.

Table 1: TraceCERT^® calibration standards for IC

Cat. No.	Product Name	Concentration (mMole)	Example Certificate
50972	2,6-pyridinedicarboxylic acid	20
50433	DL-tartaric acid	100
55517	Methanesulfonic acid	100
16355	Nitric acid	100
50439	Perchloric acid	10
61699	Potassium hydroxide	100
36486	Sodium bicarbonate	100
56169	Sodium carbonate	100
43617	Sodium hydroxide	100
68279	Sulfuric acid	100
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Packaging: 1L HDPE bottles with 45mm screw thread

Fluka has developed 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 new product 00612 is available in 2.5L and 5L package size and specified as follows:


Organic Traces:
Acetate, formiate, glycolate, oxalate: ≤ 10 µg/kg each

Cation Traces:
Al, Ba, Bi, Cd, Co, Cr, Cu, Fe, Li, Mg, Mn, Mo, Ni, Pb, Sr, Zn: ≤ 5 ìg/kg each Ca, K, Na: ≤ 10 µg/kg
each NH4+: ≤ 50µg/kg

Anion Traces:
Bromide, chloride, fluoride, iodide, nitrate, nitrite, phosphate, sulfate: 1 µg/kg each

Conductivity:
≤ 2 µS/cm

Ion chromatographic standard solutions require slightly different specification than spectroscopic solutions:

• The solution is filtered through a 0.45 mm membrane filter to prevent the column from clogging
• pH > 3

All the solutions are carefully prepared from high-purity salts, preferably nitrates; their concentration is 1000 mg/L. For packaging high-density polyethylene bottles are used. On each label the expiry date of the solution is stated.

Cation Standards for Ion Chromatography (1000mg/L)

Anion Standards for Ion Chromatography (1000 mg/L)

Multiion Standards for Ion Chromatography

Eluent Concentrates for Ion Chromatography

Organic Acid Standards for Ion Chromatography (1000mg/L)

Due to the omnipresence of organic acids in foods and beverages such as fruit drinks and wines and their link to certain nutritional, quality and safety aspects of the food, interest in measuring their concentration is growing rapidly. Ion chromatography is a common method for the analysis of organic acids.

To meet the requirements of our analytical customers, we developed a group of organic acids standards for ion chromatography (Table 1). The concentration is 1.000 g/L in water. All standards are carefully prepared from high purity starting materials, dissolved in water 17749 for analytical usage, filtered through a 0.22µm membrane filter to prevent column fouling and clogging. All standards packaged in high density polyethylene bottles under sterile conditions. An expiration date is clearly provided on each bottle.

Catalog No.	Brand	IC Standard
13669	Fluka	Acetate
38730	Fluka	Citrate
49897	Fluka	Formate
49323	Fluka	Malonate
04621	Fluka	Oxalate
04924	Fluka	Phthalate
02717	Fluka	Propionate
50824	Fluka	Tartrate
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IC standards supplied in 100 mL HDPE bottles.

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