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Poster # 240-8P Results and Discussion Conclusions Results and Discussion – Extended Analysis Speeding Up Your Natural Gas Analysis Using a Micro GC Natural Gas Analyzer Remko van Loon and Coen Duvekot, Micro GC Product Marketing, Agilent Technologies, Middelburg, the Netherlands Introduction To learn more about the Agilent 490 Micro GC Natural Gas Analyzer visit www.agilent.com/chem/microgc [1] 5991-0275EN; Application Note – Fast Analysis of Natural Gas Using the Agilent Natural Gas Analyzer; 2012. [2] 5991-0301EN; Data Sheet – Agilent 490 Micro GC Natural Gas Analyzers; 2012. [3] 5991-1093EN; Brochure – Agilent Analyzers and Application Kits; October 2012. Leave your business card for a reprint of this poster. Open a QR code application on your smart phone a scan for more info. This poster shows fast analysis of natural gas using the Micro GC based Natural Gas Analyzer (Figure 1). The Micro GC can be equipped with one to four independent column channels. Each column channel is a complete, miniaturized GC with electronic carrier gas control, micro-machined injector, narrow-bore analytical column and micro thermal conductivity detector (μTCD). References Micro GC based analyzer can be used for fast and accurate analysis of natural gas and related streams; baseline separation for all compounds of interest is obtained. Micro GC Natural Gas Analyzers are shipped as a total solution, including reporting tools for calorific value calculations. Fast analysis of natural gas is achieved on two channel Micro GC containing a PLOT U and CP-Sil 5 column; typical analysis time up to n-C8 is 200 seconds. Additional information about the permanent gases is obtained by an optional third channel with a MolSieve 5A column. The back flush functionality ensures that the undesired compounds will not enter the analytical column, which results in the protection of the column and shorter analysis times. Metal surface deactivation (UltiMetal) of Micro GCs’ sample inlet results in excellent peak shape for hydrogen sulfide. Pre-configured, factory-tested and ready to perform your analysis Rugged, compact, laboratory-quality analysis When and where you need it – on the lab, in the field or on-line Results in seconds - when speed matters Micro GC Natural Gas Analyzers Figure 1. Micro GC based Natural Gas Analyzers. Results and Discussion – Natural Gas Analysis Column temperature 80 °C Carrier gas argon, 200 kPa Injection time 40 ms Back flush time 11 sec Figure 4. Permanent gases in natural gas separated on MolSieve column. Figure 3. Chromatogram for natural gas on 6 meter Sil 5 CB column. 0 30 60 90 120 150 180 210 Seconds Zoom 6 Peak identification 1 i-butane 5 n-pentane 2 n-butane 6 n-hexane 3 neo-pentane 7 n- heptane 4 i-pentane 8 n-octane 1 2 3 4 5 7 8 PLOT U column for methane – air separation The first column channel is equipped with a PoraPLOT U analytical column for the separation of methane from the composite air peak and show also baseline separation for carbon dioxide, ethane, hydrogen sulfide and propane (Figure 2). Inert sample path for hydrogen sulfide analysis The sample inlet of the Micro GC have been treated with a metal surface deactivation process (UltiMetal), which results in an inert sample flow path and excellent peak shape for hydrogen sulfide (Figure 2), even at low concentrations. Back flush to speed up analysis time Hydrocarbons above propane, present in natural gas, were back flushed to improve analysis time. A back flush Micro GC channel consists of a pre-column and an analytical column; the two columns are coupled at a pressure point. This setup enables the possibility to invert the carrier gas flow direction through the pre-column at any time. As a result the undesired compounds will not enter the analytical column and send to vent. 15 30 45 60 75 Seconds Zoom Peak identification 1 composite air peak 2 methane 3 carbon dioxide 4 ethane 5 hydrogen sulfide 6 propane 1 2 3 4 5 4 5 3 6 6 Zoom Column temperature 60 °C Carrier gas helium, 175 kPa Injection time 40 ms Back flush time 17 sec Figure 2. Chromatogram for natural gas on PLOT U column. Natural Gas Analyzer characteristics Analyzer A Analyzer A Extended Analyzer B Analyzer B Extended Column channels installed HayeSep A CP-Sil 5 CB, 6m HayeSep A CP-Sil 5 CB, 4m CP-Sil 5 CB, 8m PoraPLOT U CP-Sil 5 CB, 6m CP-MolSieve 5A PoraPLOT U CP-Sil 5 CB, 6m Hydrocarbons (up to C9) (up to C12) (up to C9) (up to C9) Carbon dioxide Hydrogen sulfide Composite air Permanent gases (N 2 , O 2 , He & H 2 ) Typical analysis time 100 s (up to C7) 200 s (up to C8) 400 s (up to C9) 100 s (up to C7) 200 s (up to C8) 240 s (up to C12) 75 s (up to C7) 200 s (up to C8) 400 s (up to C9) 75 s (up to C7) 200 s (up to C8) 400 s (up to C9) In total, four analyzer configurations are available for the analysis of natural gas. Setup of these analyzers depenends on analysis requirements; column choice and analysis characteristics are shown in table below. For this poster the Natural Gas Analyzer B and B Extended were used. Additionally, a micro gasifier accessory was used to expand the application range to liquified natural gas (LNG). Instrument Setup 0 15 30 45 60 75 Seconds Peak identification 1 helium 2 hydrogen 3 oxygen 4 nitrogen 5 methane 1 2 3 4 5 Zoom Molecular Sieve column for permanent gas analysis The Extended Natural Gas Analyzer, equipped with an additional column channel containing a molecular sieves, is used when detailed information about the permanent gases in natural is needed. Figure 4 shows the chromatogram for this channel using argon carrier gas. Back flush to protect analytical column Moisture and carbon dioxide tend to adsorb quickly to the molsieve stationary phase and change its chromatographic properties. This would results, over time, in retention shifts and loss of separation; to maintain the separation efficiency of this column, these compounds are back flushed. Reporting tools for physical properties Physical properties, such as heating value and wobbe index, are calculated conform official methods from American Society of Testing and Materials (ASTM), Gas Processors Association (GPA) and International Standards Organization (ISO). Column temperature 70 °C Carrier gas helium, 150 kPa Injection time 40 ms C4+ hydrocarbons analyzed on a second column channel Simultaneously, butanes and higher hydrocarbons are analyzed on a second column channel equipped with a 6 meter CP-Sil 5 CB column. Analysis up to C8 is done was done in just over 3 minutes as depicted in Figure 3.

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Page 1: Poster # 240-8P...Leave your business card for a reprint of this poster. Open a QR code application on your smart phone a scan for more info. This poster shows fast analysis of natural

Poster # 240-8P

Results and Discussion

Conclusions

Results and Discussion – Extended Analysis

Speeding Up Your Natural Gas Analysis Using a Micro GC Natural Gas Analyzer Remko van Loon and Coen Duvekot, Micro GC Product Marketing, Agilent Technologies, Middelburg, the Netherlands

Introduction

To learn more about the Agilent 490 Micro GC Natural Gas Analyzer visit www.agilent.com/chem/microgc [1] 5991-0275EN; Application Note – Fast Analysis of Natural Gas Using the Agilent Natural Gas Analyzer; 2012. [2] 5991-0301EN; Data Sheet – Agilent 490 Micro GC Natural Gas Analyzers; 2012. [3] 5991-1093EN; Brochure – Agilent Analyzers and Application Kits; October 2012. Leave your business card for a reprint of this poster. Open a QR code application on your smart phone a scan for more info.

This poster shows fast analysis of natural gas using the Micro GC based Natural Gas Analyzer (Figure 1). The Micro GC can be equipped with one to four independent column channels. Each column channel is a complete, miniaturized GC with electronic carrier gas control, micro-machined injector, narrow-bore analytical column and micro thermal conductivity detector (μTCD).

References

• Micro GC based analyzer can be used for fast and accurate analysis of natural gas and related streams; baseline separation for all compounds of interest is obtained.

• Micro GC Natural Gas Analyzers are shipped as a total solution, including reporting tools for calorific value calculations.

• Fast analysis of natural gas is achieved on two channel Micro GC containing a PLOT U and CP-Sil 5 column; typical analysis time up to n-C8 is 200 seconds.

• Additional information about the permanent gases is obtained by an optional third channel with a MolSieve 5A column.

• The back flush functionality ensures that the undesired compounds will not enter the analytical column, which results in the protection of the column and shorter analysis times.

• Metal surface deactivation (UltiMetal) of Micro GCs’ sample inlet results in excellent peak shape for hydrogen sulfide.

Pre-configured, factory-tested and ready to perform

your analysis

Rugged, compact, laboratory-quality

analysis

When and where you need it – on the lab, in the field or on-line

Results in seconds - when speed matters

Micro GC Natural Gas Analyzers

Figure 1. Micro GC based Natural Gas Analyzers.

Results and Discussion – Natural Gas Analysis

Column temperature 80 °C Carrier gas argon, 200 kPa Injection time 40 ms Back flush time 11 sec Figure 4. Permanent gases in natural gas separated on MolSieve column.

Figure 3. Chromatogram for natural gas on 6 meter Sil 5 CB column.

0 30 60 90 120 150 180 210Seconds

Zoom

6

Peak identification 1 i-butane 5 n-pentane 2 n-butane 6 n-hexane 3 neo-pentane 7 n- heptane 4 i-pentane 8 n-octane

1 2 3

4 5

7 8

PLOT U column for methane – air separation

The first column channel is equipped with a PoraPLOT U analytical column for the separation of methane from the composite air peak and show also baseline separation for carbon dioxide, ethane, hydrogen sulfide and propane (Figure 2). Inert sample path for hydrogen sulfide analysis The sample inlet of the Micro GC have been treated with a metal surface deactivation process (UltiMetal), which results in an inert sample flow path and excellent peak shape for hydrogen sulfide (Figure 2), even at low concentrations. Back flush to speed up analysis time Hydrocarbons above propane, present in natural gas, were back flushed to improve analysis time. A back flush Micro GC channel consists of a pre-column and an analytical column; the two columns are coupled at a pressure point. This setup enables the possibility to invert the carrier gas flow direction through the pre-column at any time. As a result the undesired compounds will not enter the analytical column and send to vent.

15 30 45 60 75Seconds

Zoom

Peak identification 1 composite air peak 2 methane 3 carbon dioxide 4 ethane 5 hydrogen sulfide 6 propane

1

2

3

4

5

4 5

3 6

6

Zoom

Column temperature 60 °C Carrier gas helium, 175 kPa Injection time 40 ms Back flush time 17 sec Figure 2. Chromatogram for natural gas on PLOT U column.

Natural Gas Analyzer characteristics

Analyzer A Analyzer A Extended

Analyzer B Analyzer B Extended

Column channels installed • HayeSep A • CP-Sil 5 CB, 6m

• HayeSep A • CP-Sil 5 CB, 4m • CP-Sil 5 CB, 8m

• PoraPLOT U • CP-Sil 5 CB, 6m

• CP-MolSieve 5A • PoraPLOT U • CP-Sil 5 CB, 6m

Hydrocarbons (up to C9) (up to C12) (up to C9) (up to C9) Carbon dioxide Hydrogen sulfide Composite air Permanent gases (N2, O2, He & H2) Typical analysis time 100 s (up to C7)

200 s (up to C8) 400 s (up to C9)

100 s (up to C7) 200 s (up to C8) 240 s (up to C12)

75 s (up to C7) 200 s (up to C8) 400 s (up to C9)

75 s (up to C7) 200 s (up to C8) 400 s (up to C9)

In total, four analyzer configurations are available for the analysis of natural gas. Setup of these analyzers depenends on analysis requirements; column choice and analysis characteristics are shown in table below. For this poster the Natural Gas Analyzer B and B Extended were used. Additionally, a micro gasifier accessory was used to expand the application range to liquified natural gas (LNG).

Instrument Setup

0 15 30 45 60 75Seconds

Peak identification 1 helium 2 hydrogen 3 oxygen 4 nitrogen 5 methane

1

2

3 4

5

Zoom

Molecular Sieve column for permanent gas analysis The Extended Natural Gas Analyzer, equipped with an additional column channel containing a molecular sieves, is used when detailed information about the permanent gases in natural is needed. Figure 4 shows the chromatogram for this channel using argon carrier gas. Back flush to protect analytical column Moisture and carbon dioxide tend to adsorb quickly to the molsieve stationary phase and change its chromatographic properties. This would results, over time, in retention shifts and loss of separation; to maintain the separation efficiency of this column, these compounds are back flushed. Reporting tools for physical properties Physical properties, such as heating value and wobbe index, are calculated conform official methods from American Society of Testing and Materials (ASTM), Gas Processors Association (GPA) and International Standards Organization (ISO).

Column temperature 70 °C Carrier gas helium, 150 kPa Injection time 40 ms

C4+ hydrocarbons analyzed on a second column channel Simultaneously, butanes and higher hydrocarbons are analyzed on a second column channel equipped with a 6 meter CP-Sil 5 CB column. Analysis up to C8 is done was done in just over 3 minutes as depicted in Figure 3.