Agilent Technologies 490 Bedienungsanleitung

Agilent 490 

Micro GC Biogas

Analyzers

User Manual

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Manual Part Number

G3582-90000

Edition

Second edition, February 2012

Printed in USA

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Agilent 490 Micro GC Biogas Analyzers

User Manual

Agilent Technologies

The Agilent Biogas Analyzers

Biogas is a type of biofuel produced by the biological breakdown

of organic material in an anaerobic environment. The anaerobic

digestion or fermentation process of biodegradable materials

such as manure, sewage, municipal waste, green waste, plant

material, or crops produces biogas. Biogas is composed of

methane, carbon monoxide, hydrogen, carbon dioxide, nitrogen,

hydrogen sulfide, and oxygen. When methane, hydrogen, and

carbon monoxide are combusted or oxidized with oxygen,

energy is produced that can be used as fuel.

The Agilent 490 Micro GC Biogas Analyzer is a factory tuned

analyzer specific for biogas analysis.

Two types of Biogas Analyzers are available: Agilent 490 Micro

GC Biogas Analyzer and the Agilent 490 Micro GC Biogas

Analyzer Extended. The choice of configuration depends on the

type of biogas sample.

Biogas Analyzer

The Agilent 490 Micro GC Biogas Analyzer is used to analyze

pure biogas including analysis of permanent gases, hydrogen

sulfide and hydrocarbons up to n-propane. This is a dual

cabinet equipped with a CP-Molsieve 5A channel and a

CP-PoraPLOT U channel with dual carrier gas option.

Biogas Analyzer Extended

The Agilent 490 Micro GC BiogasFirst edition, December 2011

Analyzer Extended is used to analyze biogas mixed with other

hydrocarbon streams. The analysis consists of permanent gases,

hydrogen sulfide and hydrocarbons up to n-heptane. The Biogas

Analyzer Extended is a quad cabinet equipped with three

channels: a CP-Molsieve 5A, a CP-PoraPLOT U channel and a

CP-Sil 5 CB channel with dual carrier gas option.

Before starting up the Analyzer make sure that correct carrier

gases are connected for all channels. Argon carrier gas is

required for the CP-Molsieve channel and Helium for all other

channels. The required pressure for all carrier gases is 550 kPa

(80 psi). More detail concerning the Agilent Micro GC can be

found in the Agilent 490 Micro GC user manual.

4Biogas Analyzers

The Agilent Biogas Analyzers

Checkout information

The Biogas Analyzer is factory tuned including appropriate

settings for backflush times for the CP- Molsieve 5A and

CP-PoraPLOT U channel. Final checkout of the Agilent 490

Micro GC Biogas Analyzers is performed with a Universal Gas

Calibration standard. This contains helium, neon, hydrogen,

oxygen, nitrogen, methane, ethane, ethylene, carbon dioxide,

carbon monoxide, acetylene, n-propane, methyl acetylene and

n-butane. Not all components of this Calibration Standard are

specified for the Biogas Analyzers. This calibration standard is

used as a reference for the performance of the Biogas Analyzer.

For more details regarding the Universal Gas Calibration

Standard, see Appendix 1.

The Universal Gas Calibration Standard is shipped with the

Analyzer and will be used by the Agilent Customer Engineer at

installation. The factory tuned method, final chromatogram

(Test Report) and this Biogas Analyzer user manual are

supplied with the Biogas Analyzer on the analyzer CD.

Use the Universal Gas Calibration Standard to perform

reference checks on the Biogas Analyzer. Load the method from

the Analyzer CD if Openlab CDS EZChrom Edition is used or

create a method using the settings from the method PDF file on

the Analyzer CD. For a quick start, see Appendix 2. Connect and

inject the Calibration Standard.

The Universal Gas Calibration Standard does not contain

hydrogen sulfide, neo-pentane, n-pentane or i-pentane. For

these components, reference chromatograms are included in

this manual.

The Agilent Biogas Analyzers

Biogas Analyzers 5

CP-Molsieve channel

The CP-Molsieve 5A channel of the Biogas Analyzer analyzes

permanent gases such as helium, neon, hydrogen, oxygen,

nitrogen, methane and carbon monoxide.

Figure 1 is a chromatogram of the Universal gas Calibration

Standard analyzed on the CP-Molsieve 5A channel.

Figure 1 The Universal Gas Calibration Standard analyzed on the CP-Molsieve channel

Seconds

20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110

Helium

Neon

Hydrogen

Oxygen

Nitrogen

Methane

Carbon Monoxide

6Biogas Analyzers

The Agilent Biogas Analyzers

CP-PoraPLOT U channel

The CP-PoraPLOT U channel of the Biogas Analyzer is used to

analyze carbon dioxide, ethane, hydrogen sulfide and

n-propane. This channel and the sample inlet are Ultimetal

deactivated which results in improved performance for

hydrogen sulfide analysis.

The chromatogram obtained from the Universal Gas Calibration

Standard with the CP-PoraPLOT U is shown in Figure 2.

If a sample contains hydrogen sulfide, the chromatogram

resembles Figure 3.

Figure 2 The Universal Gas Calibration Standard analyzed on the CP-PoraPLOT U channel

Figure 3 A mixture with hydrogen sulfide analyzed on the CP-PoraPLOT U channel

Seconds

20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50

0.5

1.0

1.5

2.0

2.5

Composite Air Peak

Carbon Dioxide

Ethylene

Ethane

Acetylene

n-Propane

Seconds

22 24 26 28 30 32 34 36 38 40 42 44 46 48 50

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1.0

1.1

Composite Air Peak

Carbon Dioxide

Ethylene

Ethane

Acetylene

Hydrogen Sulfide

n-Propane

The Agilent Biogas Analyzers

Biogas Analyzers 7

CP Sil 5 CB channel

The CP-Sil 5 CB channel of the Biogas Analyzer Extended is

used to analyze the hydrocarbon up to n-heptane. Hydrocarbons

that are specified for this analyzer are i-butane, n-butane,

neo-pentane, n-pentane, iso-pentane, n-hexane, and n-heptane.

The Universal Gas Calibration Standard does not contain all

these hydrocarbons. A reference chromatogram is included in

this manual for the missing components.

Analyzing the Universal Gas Calibration Standard with the

CP-Sil 5 CB results in the chromatogram shown in Figure 4.

If a hydrocarbon mixture up to n-hexane is used, the

chromatogram resembles Figure 5.

Figure 4 The Calibration Standard analyzed on CP-Sil 5 CB channel

Figure 5 A hydrocarbon mixture up to n-Hexane analyzed on the CP-Sil 5 CB channel

Seconds

10 20 30 40 50 60 70 80 90 100 110 120 130

n-Propane

Methyl Acetylene

n-Butane

n-Hexane

n-Heptane

Seconds

15 20 25 30 35 40 45 50 55 60

100

150

200

250

300

Composite Air peak

Ethane

n-Propane

i-Butane

n-Butane

neo-Pentane

n-Pentane

i-Pentane

n-Hexane

8Biogas Analyzers

The Agilent Biogas Analyzers

Tuning the backflush time

For the CP-Molsieve 5A and the CP-PoraPLOT U channel, the

backflush times must be tuned. For tuning, the Universal Gas

Calibration Standard is recommended.

The purpose of tuning the CP-Molsieve 5A is to get all methane

on the column while all components such as moisture, carbon

dioxide, ethane and higher hydrocarbons are backflushed. The

CP-PoraPLOT U is tuned on the n-Propane peak while all other

hydrocarbons that elute after it are backflushed.

1Set the backflush time at 0 second and analyze the

Calibration standard. The purpose of this is to identify the

components in the Standard.

2Change the backflush time. Start with 10 seconds and make

a run. Now the following can be observed:

•When the backflush time is set too early you will see the

peak of interest partially or totally backflushed.

•If the backflush time is set too late the unwanted

components are not backflushed.

3Adjust the backflush time until a huge difference is noticed

in the peak of interest. Then make smaller steps (0.1

seconds) until the optimal backflush time is found.

Figure 6 shows a simple example of tuning the backflush time

for the CP-Molsieve 5A channel.

Figure 6 Effect of backflush time on the peak of interest

Backﬂush Time (s)

Tuning Backﬂush for CP-Molsieve channel

Area_peak of interest

910 11 12 13

The Agilent Biogas Analyzers

Biogas Analyzers 9

Appendix 1: Certificate of the Universal Gas Calibration Standard

Part No: 5184-3541 Part No. Kit: 5184-3546

10 Biogas Analyzers

The Agilent Biogas Analyzers

Appendix 2: The Biogas Analyzer method

For more details of the method see the PDF method file

available on the analyzer CD.

The backflush time must be tuned for each new CP-Molsieve and

CP-PoraPLOT channel.

Tabl e 1 The Biogas Analyzer method

Method Settings CP-Molsieve 5A CP-PoraPLOT U CP-Sil 5 CB

Carrier gas Argon Helium Helium

Injector Temperature (°C) 110 110 110

Injection Time (ms) 40 40 40

Backflush time (s) 11 14 -

Column Temperature (°C) 80 80 60

Pressure (kPa) 200 150 150

Sample Line temperature (°C) 110 110 110

Invert signal Yes No No

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