Page 42 - Application Handbook - TOC
P. 42

Sum parameter – Total Organic Carbon




                                         TOC – Determination in sodium nitrate
                                         and sodium nitrite
                    SCA-130-308


            Basic chemicals may contain organic
            contaminants influencing the quality of              Compound
            products. Quality control procedures of the           (Concen-           Dilution         Conz.
            reactants are, therefore, necessary in order to        tration)      Weighted Sample
            detect impurities.                                                      5 g / 50 ml      approx.
                                                                Sodium nitrate     add. 1-2 drops      10%
            For     the    determination    of    organic          (>99,9%)       Sulfuric acid until
            contaminations in salts, solutions of these                                pH<7
            salts  can  be prepared and subsequently                             Weighted Sample
                                                                                    5 g / 50 ml
            measured using a TOC-L analyzer.                                       add. 1-2 drops
                                                                                                     approx.
                                                                 Sodium nitrite    Sulfuric acid until   10%
                                                                   (>99,9%)            pH<7
                                                                                 Caution: Nitrogen
                                                                                   oxide gas is
                                                                                     released


                                                                Caution: Nitrite salts react to form of toxic
                                                                nitrous gases. Sample preparation should,
                                                                therefore, always be carried out  under a
                                                                hood. The samples should only be  removed
                                                                from the hood, when no more nitrous gases
                                                                escape.

                                                                Calibration of the TOC-L system  was done
            High salt  concentrations generally present a       applying the automatic dilution function in the
            problem for TOC analysis. These  salts  can         range of 0.5 mg/L to 10 mg/L.
            crystallize in the combustion system and lead
            to higher maintenance needs.

            In the case described below, the NPOC
            content of  two salts  was determined. The
            difficulty was the required detection limit of 10
            mg/kg.


            ■ Sample preparation
            For sample preparation, 5 g of  both salts
            (sodium nitrite and sodium nitrate) were                        Fig. Multi-point calibration
            weighed into a 50 mL volumetric flask  and                       with dilution function
            diluted with ultrapure  water. During dilution,
            the solutions were acidified with concentrated
            sulfuric acid (25%).
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