Determination of Argon in Ammonia Plant Process Gas Streams by Gas Chromatography
Upcoming SlideShare
Loading in...5
×
 

Determination of Argon in Ammonia Plant Process Gas Streams by Gas Chromatography

on

  • 743 views

Determination of Argon in Ammonia Plant Process Gas Streams by Gas Chromatography ...

Determination of Argon in Ammonia Plant Process Gas Streams by Gas Chromatography

SCOPE AND FIELD OF APPLICATION

This document is a method for the determination of argon in process gas streams in the range 0-10% v/v.

Statistics

Views

Total Views
743
Slideshare-icon Views on SlideShare
743
Embed Views
0

Actions

Likes
0
Downloads
15
Comments
0

0 Embeds 0

No embeds

Accessibility

Upload Details

Uploaded via as Adobe PDF

Usage Rights

© All Rights Reserved

Report content

Flagged as inappropriate Flag as inappropriate
Flag as inappropriate

Select your reason for flagging this presentation as inappropriate.

Cancel
  • Full Name Full Name Comment goes here.
    Are you sure you want to
    Your message goes here
    Processing…
Post Comment
Edit your comment

    Determination of Argon in Ammonia Plant Process Gas Streams by Gas Chromatography Determination of Argon in Ammonia Plant Process Gas Streams by Gas Chromatography Document Transcript

    • GBH Enterprises, Ltd. Plant Analytical Techniques GAS ANALYSIS: Determination of Argon in Ammonia Plant Process Gas Streams by Gas 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
    • Gas Analysis: 1 Determination of Argon in Ammonia Plant Process Gas Streams by Gas Chromatography SCOPE AND FIELD OF APPLICATION This document is a method for the determination of argon in process gas streams in the range 0-10% v/v. 2 PRINCIPLE The gas sample will be injected automatically by a ten port valve onto the poraplot U column. The unsplit hydrogen, argon, nitrogen, methane and carbon monoxide will elute first and be switched to the mole sieve column. The molsieve column will be isolated and the poraplot column will elute any carbon dioxide and ethane present via a restrictor column to the detector. After the elution of the carbon dioxide and ethane the poraplot column will be back flushed to remove any C3 and higher hydrocarbons from the system. Then the separated hydrogen, argon, nitrogen, methane and carbon monoxide will be allowed to elute from the mole sieve column (see figure 1). A micro T.C.D. is used which depends on keeping one resistance filament as a reference and the second as an analyzer resistance filament. 3 MATERULSRFQUIRED 3.1 Carrier Gas 3.1.1 Helium at not less than 100 kpa pressure. 3.2 Materials for the Preparation of Standards 3.2.1 Argon 3.2.2 Hydrogen HYDROGEN IS EXPLOSIVE WHEN MIXED WITH AIR AT CONCENTRATION RANGING APPROXIMATELY FROM 4% TO 75% (V/V). CHECK FOR LEAKS. 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 APPARATUS 4.1 General Description 4.1.1 Gas chromatographic system, the system comprises a gas chromatograph with a thermistor detector. A chrompack 9000 G.C. is suitable. 4.1.2 Characteristics of the Assembly 4.1.2.1 Column temperature, isothermal temperature control range 30°C-50°C to within + 0.50oC. 4.1.2.2 Detector temperature, should be within the range 80oC-120oC to within +0.50oC. 4.1.3 Gas Controls and Flow Measurement 4.1.3.1 Pressure regulators, supplied by manufacturers of the gas chromatographic equipment. 4.1.3.2 Bubble flow meter, which can be used over a range of 0.1 to 50ml/MIN. 4.2 Injection Equipment 4.2.1 Injection system comprising a ten port gas sampling valve with a 50 µl sample loop. 4.3 Columns 4.3.1 Three columns are required. 4.3.1.1 Poraplot U Column (Quartz/Capillary) 10 m x 0.32mm t 5 m x 0.32 mm (Particle/Trap). 4.3.1.2 Mole sieve Column (Quartz Capillary). 4 m x 0.32mm t 2 5 m x 0.32mm deactivated fused silica. 4.3.1.3 Restriction Capillary Column. 10 m x 0.32mm deactivated fused silica. 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
    • 4.3.2 Conditioning 4.3.2.1 The mole sieve column is conditioned by passing helium through the column for 12 hours with the oven set at 17OoC. 4.3.3 Resolution There shall be full resolution from peak height to base line between all peaks as shown on the typical chromatograph (see Figure 2). 4.4 Detector The micro thermal conductivity detector is a dual channel device with a reference flow of carrier gas through the second channel. The detector measures the difference in thermal conductivity between two gas streams when a sample passes through one of the channels. Make-up gas is required. 4.5 Recorder Having the following characteristics. 4.5.1 Suitable for a chart speed of l0 mm/min. 4.5.2 Single span lmv measuring range. 5 SAMPLE 5.1 The gas sample to be analyzed is collected in glass aspirator bottles. (See sampling procedure S3/1/1). 5.2 Preparation of Test Portions Approximately lOOm1 of the sample shall be purged through the sample loop, before turning the sample into the chromatograph. 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 PROCEDURE 6.1 Setting up the Apparatus 6.1.1 Oven and Columns 6.1.1.1 Oven Temperature - 40°C. 6.1.1.2 Detector Temperature 100°C 6.1.1.3 Helium Carrier. P.l. Pressure 70 KPA P.2. Pressure 45 KPA P.3. Pressure 45 KPA 6.1.1.4 Helium Carrier to detector 4.5ml/min. 6.1.1.5 Helium Carrier M.U.G. 45 ml/min. 6.2 Calibration 6.2.1 Calibrate by external calibration. 6.2.2 Standard mixtures. 6.2.2.1 Purity of components. The purity of the gases used to make standard blends shall not be less than 99.5% 6.2.2.2.1 Calibration gas mixtures are produced using a gas blending instrument, a Wosthoff Gas proportioning pump or a signal gas blender are suitable. The composition of the calibration mixtures % v/v is: Argon 5% Argon 10% Hydrogen 95% Hydrogen 90% (HYDROGEN BEING THE LARGEST COMPONENT OF THE PROCESS GAS TO BE ANALYZED). 6.2.2.2 The calibration mixtures are passed directly into the sample loop (see 5.2). 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
    • 6.2.3 Presentation of the calibration data. The calibration results are presented in the form of a graph. (Figure 3 and Figure 4). 6.3 Test 6.3.1 Preparation of the Test Portion Collect gas sample as described in (5.1). 6.3.2 Introduction of the Test Portion Purge 100 ml of sample through the 10 port valve, with the valve set in the purge position. Disconnect the sample bottle, then turn the valve to the sample position. 6.4 Examination of the Chromatogram 6.4.1 A typical chromatogram for the analysis is shown in Figure 2. 6.4.2 Identification The argon is identified by comparing the retention times of the sample chromatogram against the argon standard retention time. 6.4.3 Quantitative Analysis Calculate the amount of argon by using the graph. Draw in the peak base and measure the peak height in mm and read the %v/v directly from the graph. 7 EXPRESSION OF RESULTS 7.1 The concentration of the gas analysed as a percentage by volume, to the nearest 0.1%. 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
    • 8 REPEATABILITY The following data was obtained by the analysis of gas samples produced on a proportioning pump (see 6.2.2.2.1). Injection No. 1 2 3 4 5 6 7 8 9 10 6.0 6.0 6.0 6.0 6.1 6.1 6.0 6.0 6.1 6.1 %An. 11 12 13 14 15 16 17 18 19 20 6.0 6.0 6.0 5.9 6.0 6.0 6.0 6.0 6.0 6.0 MEAN STD DEVIATION % RSD 6.015 0.049 0.8 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
    • 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
    • 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
    • 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
    • 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