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GBH Enterprises, Ltd.

Plant Analytical Techniques
ANHYDROUS AMMONIA: DETERMINATION OF ANIONS BY ION
CHROMATOGRAPHY

Infor...
AMMONIA SOLUTION: Determination of Anions (Cl, PO,, NO, b SO,) by Ion
Chromatography
WARNING AND SAFETY PRECAUTIONS:
AMMON...
3.2

Preparation of calibration solution, pipette 10 ml of standard stock
anion solution (3.1), using a Grade A 10 ml pipe...
4.5

Platinum evaporating dish.

4.6

Steam bath.

5

Sample Pretreatment

5.1

Transfer a volume equivalent to 100 g of t...
7

Expression of Results

7.1 The results are expressed as Cl, NO, PO, and SO, ppm m/v.

Refinery Process Stream Purificat...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
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Determination of Anions by Ion Chromatography

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Determination of Anions by Ion Chromatography

1 SCOPE AND FIELD OF APPLICATION

This method is suitable for the determination of inorganic anions in Ammonia Solution in the range 100 ppb to 50 ppm m/v.

2 PRINCIPLE

The sample is passed through a column of anion exchange resin, on which the anions are absorbed and separated. They are then eluted with dilute sodium carbonate/sodium hydrogen carbonate solution and passed through a suppressor. This replaces the cations with hydrogen ions and thus reduces the background conductivity of the eluent. Final measurement is by conductivity

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Transcript of "Determination of Anions by Ion Chromatography"

  1. 1. GBH Enterprises, Ltd. Plant Analytical Techniques ANHYDROUS AMMONIA: DETERMINATION OF ANIONS BY ION CHROMATOGRAPHY Information contained in this publication or as otherwise supplied to Users is believed to be accurate and correct at time of going to press, and is given in good faith, but it is for the User to satisfy itself of the suitability of the information for its own particular purpose. GBHE gives no warranty as to the fitness of this information for any particular purpose and any implied warranty or condition (statutory or otherwise) is excluded except to the extent that exclusion is prevented by law. GBHE accepts no liability for loss or personnel injury caused by or resulting from reliance on this information. Freedom under Patent, Copyright and Designs cannot be assumed. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com
  2. 2. AMMONIA SOLUTION: Determination of Anions (Cl, PO,, NO, b SO,) by Ion Chromatography WARNING AND SAFETY PRECAUTIONS: AMMONIS SOLUTION: SPLASHES INT0 EYES CAN CAUSE SEVERE BURNS. AVOID INGESTION. PRESSURE MAY BUILD UP IN CLOSED CONTAINERS. 1 SCOPE AND FIELD OF APPLICATION This method is suitable for the determination of inorganic anions in Ammonia Solution in the range 100 ppb to 50 ppm m/v. 2 PRINCIPLE The sample is passed through a column of anion exchange resin, on which the anions are absorbed and separated. They are then eluted with dilute sodium carbonate/sodium hydrogen carbonate solution and passed through a suppressor. This replaces the cations with hydrogen ions and thus reduces the background conductivity of the eluent. Final measurement is by conductivity. 3 Reagents During the analysis use only reagents of analytical reagent grade, unless otherwise specified, and water which has been deionized and then distilled from an all glass apparatus, or water of equivalent purity. 3.1 Standard stock anion solution, weigh respectively 0.4125 g sodium Chloride, 0.7164 g potassium dihydrogen phosphate, 0.6853 g sodium nitrate and 0.9075 g potassium sulfate and transfer to a 500 ml one mark volumetric flask add approximately 300 ml water. Shake until dissolution is complete, dilute to the mark with water and mix. 1 ml of this solution contains 0.5 mg Cl, 1.0 mg PO, 1.0 mg NO, and 1.0 mg SO,. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com
  3. 3. 3.2 Preparation of calibration solution, pipette 10 ml of standard stock anion solution (3.1), using a Grade A 10 ml pipette, into a 1 liter one mark volumetric flask and dilute to the mark with water and mix. 1 ml of this solution contains 5 µg Cl, 10 µg PO,, 10 µg NO, and 10 µg SO,. 3.3 Eluent (0.0017 M NaHC03, 0.0018 M Na2CO3), weigh 0.713 + 0.001 g of sodium hydrogen carbonate and 0.955 + 0.001 g of anhydrous sodium carbonate, dissolve in water and transfer to a 5 L volumetric flask (4.1) and dilute to volume with water. SODIUM CARBONATE - IRRITATING TO EYES - DUST IS STERNUTATORY – SODIUM HYDROGEN CARBONATE MAY IRRITATE EYES AND RESPIRATORY SYSTEM IF INHALED AS DUST 3.4 Suppressor regenerant (0.025 M, H2SO4), transfer 3.5 mL of concentrated Sulfuric acid (S.G. = 1.84) into a 5 L volumetric flask containing water and dilute to volume with water. SULFURIC ACID CAUSES SEVERE BURNS TO EYES AND SKIN 4 APPARATUS 4.1 Standard volumetric glassware, class A. 4.2 Ion chromatograph system. A suitable system is a Dionex QIC model comprising a micromembrane suppressor, an AG4A guard column and AS4A sample column, a 5 µg sample loop; computing integrator, a Shimadzu C-R3A model is suitable; a 3 Slot expansion accessory, a Shimadzu C-R3A model is suitable; Automation interface supplied by Dionex; a flat-bed recorder, capable of 0 - 10 mV; Compressed air supply, at 5 p.s.i. (Figure 1 shows a schematic diagram). 4.3 Auto-sampler system, a suitable system is supplied by Dionex consisting of an autosampler with autosample vial racks. 4.4 Autosampler vials, 5 mL autosampler vials with filter caps supplied by Dionex are suitable. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com
  4. 4. 4.5 Platinum evaporating dish. 4.6 Steam bath. 5 Sample Pretreatment 5.1 Transfer a volume equivalent to 100 g of the sample into the platinum evaporating dish (4.5) and reduce the volume to approximately 5 ml on a steam bath (4.6) to remove all the ammonia. Transfer the residue to a 100 ml one mark volumetric flask, wash the platinum dish with 4 x 10 ml portions of water, adding the washings to the residue in the volumetric flask. Dilute to the mark with water and mix. 6 Procedure 6.1 Ensure that the Ion chromatagraph system (4.2), autosampler system (4.3), eluent (3.3) and suppressor regenerant (3.4) are connected in accordance with the manufacturer's instructions. 6.2 Select the method for anionic determination. The parameters are set out in Annex 1. 6.3 Fill sample vials (4.4) with anion standard (3.2) and place in the autosample vial rack on the autosampler (4.3). 6.4 Test sample, fill a sample vial (4.4) with sample and place in the autosample vial rack on the autosampler (4.3). 6.5 Repeat procedure (6.4) for the required number of test samples, 6.6 Start the run in accordance with the manufacturers instructions. The results will be recorded by the computing integrator. Figure 2 shows a typical chromatogram. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com
  5. 5. 7 Expression of Results 7.1 The results are expressed as Cl, NO, PO, and SO, ppm m/v. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com
  6. 6. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com

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