Scion Instruments 456-GC Reference guide

SCION Instruments HQ SCION Instruments NL BV

Suite 34, Livingston Business Centre, 4462, Goes,

Kirkton Road South, Livingston, Stanleyweg 4.

EH54 7FA, Scotland, UK. The Netherlands

Tel: +44 1506 300 200 Tel: +31 113 348 926

sales-eu@scioninstruments.com sales-eu@scioninstruments.com

www.scioninstruments.com www.scioninstruments.com

Revised March 2019

Reference Manual

Natgas C Analyzer

With Additional He/H

2

Channel

Scion Instruments

Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 2

Section contents

INTRODUCTION .................................................................................................................................. 3

INSTRUMENT SPECIFICATIONS ................................................................................................... 4

INSTALLATION OF COLUMNS, FLOW AND PRESSURE SETTING ...................................... 5

TUNING THE NATGAS C ANALYZER ........................................................................................... 6

OPERATION ......................................................................................................................................... 7

TROUBLE SHOOTING ........................................................................................................................ 9

STEP BY STEP................................................................................................................................... 11

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Scion Instruments Natgas C Analyzer +He/H

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Channel Reference Manual Page: 3

INTRODUCTION

Natural gas analysis commonly involves the quantitation of components up

to C5 while C6 and heavier hydrocarbons are combined and measured as a

single peak (C6+). Extending the analysis to obtain the compositional

breakdown of the C6+ group can provide valuable information.

The Natgas C Analyzer is an analytical tool principally developed for the

determination of oxygen, nitrogen, carbon dioxide, and the hydrocarbons C1

to C12. Three columns are used to accomplish the single-channel analysis of

natural gas: First a molecular sieve column for oxygen and nitrogen

separation, then a Hayesep P column for the separation of methane till

hydrogen sulfide and a capillary column for the separation of C1-C12

hydrocarbons.

The instrument is tuned during Final Test to its proper settings.

Do not change any flow or pressure settings unless it is

requested.

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Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 4

INSTRUMENT SPECIFICATIONS

Every instrument is fully tested; the results of the tests, as well as the

methods used during these tests, are presented as part of this manual (refer

to section 1).

START UP

At initial START-UP as well as after a longer idle period,

follow the instructions below:

• Connect all the gases to the instrument.

• Switch the power on.

• Load the appropriate method.

• Check the flow settings.

• Condition the system as described in this manual.

• Do not make any changes to the methods.

• The system is ready for injections.

For a new system there is no need to do any flow measurement or

flow tuning before power-up. The instrument is tuned and tested in

our Factory in Goes.

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Channel Reference Manual Page: 5

INSTALLATION OF COLUMNS, FLOW AND PRESSURE SETTING

Tuning of the analyzer is only necessary in case new columns are

installed or after flow or pressure settings have been changed.

Before new columns may be installed, they need to be

preconditioned!!

Make sure, the instrument is connected to the minimum gas supply

pressures as indicated in the 400-GC series pre-installation manual.

For more detailed information concerning the configuration of the

instrument, please, refer to the drawing section (section 6 of this manual).

The factory drawing indicates which flow and pressure controls are being

used. The drawing also outlines the way the analyzer channel has been

incorporated into the gas chromatograph.

Regularly check and replace filters maintaining the supply quality as

described in the pre installation requirements.

Replacement columns

SC30128 SCION-1, 60m x 0.25mm, df = 1.0 µm

SC15919 Molsieve 13X, 4ft * 1/8", Inert Steel

SC15922 Empty delay, 10 ft * 1/8", Inert Steel

SC15920 Hayesep P, 6 ft * 1/8", Inert Steel

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Channel Reference Manual Page: 6

TUNING THE NATGAS C ANALYZER

Tuning is only necessary when new columns have to be installed or by

malfunctioning of the GC.

Connect the columns according the flow schematics given in Section 6 and

adjust the pressures (if necessary) at an oven temperature of 45°C.

Take very good care not to create any dead volume!

• Set the injection valve (V1) and the column selection valve (V2) in the (-)

position.

• While measuring the flow out the exit of the middle TCD, adjust the rear

EFC-24 flow until there is a flow of 33 ml/min.

• Set the middle EFC-24 until a flow of 27 ml/min is coming out of the vent 1.

• Set the DEFC-13 to give a flow of 30 ml/min out of the reference exit of the

TCD.

• Set the front EFC-25 pressure at 20 psi and at a split ratio of 1:200.

• Program the method as given in the OPERATION section.

• Check all connections for leakage.

After stabilization of the TCD and FID signals the system is ready for

analyses.

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OPERATION

An operational method is preloaded in the instrument.

Listed below is an example method; settings determining the application

may be different.

Sample delivery

V1 (GSV)

V2 (CS)

V4 (S)

Initial

-

0.01

- - +

0.80

-

1.00

+

-

1.91

+ + -

Injector (S/SL Front):

Temp 220 ºC

Split ratio 200

Flow/Pressure:

Front EFC-25:

Pressure (PSI)

Hold (min)

Initial:

20.0

18.00

Middle EFC-24:

Pressure (PSI)

Hold (min)

Initial:

14.0

18.00

Total Flow: 60 ml/min

Rear EFC-24:

Pressure (PSI)

Hold (min)

Initial:

12.0

18.00

Total Flow: 60 ml/min

Column Oven:

Temp(ºC)

Rate(ºC/min)

Hold(min)

Total(min)

Initial

45

--

6.00

190

20

4.75

18.00

Oven stabilization time 0.50 minutes

The temperature is raised after elution of H

2

S.

Large Valve Oven:

Temp 100 ºC

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Channel Reference Manual Page: 8

Detector (middle TCD):

Temp 200 ºC

Range 0.05

Time constant slow

Fila temp: 230 °C

Fila max: 390 °C

Polarity: negative

Autozero: yes

DEFC-13

Reference: 30 ml/min

Detector (middle FID)

Temp: 300°C

Time constant: Slow

Range : 12

Autozero: No

DEFC-11

Make-up: 30 ml/min

Hydrogen: 30 ml/min

Air 300 ml/min

Never interrupt an analytical run. The complete cycle has to

finish!

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Channel Reference Manual Page: 9

TROUBLE SHOOTING

For problems related to the basic hardware and electronics of the gas

chromatograph, as well as injectors and detectors, refer to the 400-GC

Series user manual.

In case of any analytical problem, it is always advised to record an analysis

using a reference sample. The result, including full details can be submitted

to your local Scion Instruments service department to judge performance.

Fig. 1 and fig. 2 show chromatograms of the TCD and FID tracks respectively.

In case of decreasing retention times of the Molecular Sieve column, this

column needs reconditioning. This has to be done in a different oven under

nitrogen or helium at 350° C overnight.

Check the status of the humidity filter in case of conditioning is needed. The

cause might be saturation of this filter.

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Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 10

87.576.565.554.543.532.521.510.5

650,000

600,000

550,000

500,000

450,000

400,000

350,000

300,000

250,000

200,000

150,000

100,000

50,000

0

-50,000

O2/Ar

N2

O2/Ar/N2

CH4

CO2

C2H6

H2S

RT [min]

GC0903B101_NGA-C_5_5_2009 1_02_00 PM_1_28.DATA [Middle (TCD)]

µV

Fig 1: TCD channel

1817161514131211109876543210

1,400,000

1,300,000

1,200,000

1,100,000

1,000,000

900,000

800,000

700,000

600,000

500,000

400,000

300,000

200,000

100,000

0

CH4

C2H6

C3H8

i-C4H10

n-C4H10

i-C5H12

n-C5H12

n-C6H14

RT [min]

GC0903B101_NGA-C_5_5_2009 1_02_00 PM_1_28.DATA [Rear (FID)]

µV

Fig 2: FID channel

Scion Instruments

Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 11

STEP BY STEP

Step by step customer drawings Natgas C Analyzer

Scion Instruments

Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 12

Initial Position

EFC-24

rear

Helium

Gas sample IN

Gas sample OUT

(To HeH2 channel)

Sample loop 250 µL

FID

DEFC-11

rear

TCD

DEFC-13

middle

SCION-1

SC30128

Molsieve 13X

SC15919

Empty Delay column

SC15922

Hayesep P

SC15920

Vent 1

Liquid sample IN

Liquid sample OUT

EFC-25

front

Helium

EFC-24

middle

Helium

V-4

P

C

S

W

S

LSV 5

C

P

1

2

3

4

5

6

7

8

9

10

11

12

14

13

V - 1

1

2

3

4

5

6

V - 2

Reference TCD

Helium

S/SL Injector

front

Splitvent

Permanent gases channel

Hydrocarbons C1-C16 channel

Scion Instruments

Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 13

Fill position

EFC-24

rear

Helium

Gas sample IN

Gas sample OUT

(To HeH2 channel)

Sample loop 250 µL

FID

DEFC-11

rear

TCD

DEFC-13

middle

SCION-1

SC30128

Molsieve 13X

SC15919

Empty Delay column

SC15922

Hayesep P

SC15920

Vent 1

Liquid sample IN

Liquid sample OUT

EFC-25

front

Helium

EFC-24

middle

Helium

V-4

P

C

S

W

S

LSV 5

C

P

1

2

3

4

5

6

7

8

9

10

11

12

14

13

V - 1

1

2

3

4

5

6

V - 2

Reference TCD

Helium

S/SL Injector

front

Splitvent

FILL MODE V-1 (-) V-2 (-)

Scion Instruments

Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 14

Inject position

EFC-24

rear

Helium

Gas sample IN

Gas sample OUT

(To HeH2 channel)

Sample loop 250 µL

FID

DEFC-11

rear

TCD

DEFC-13

middle

SCION-1

SC30128

Molsieve 13X

SC15919

Empty Delay column

SC15922

Hayesep P

SC15920

Vent 1

Liquid sample IN

Liquid sample OUT

EFC-25

front

Helium

EFC-24

middle

Helium

V-4

P

C

S

W

S

LSV 5

C

P

1

2

3

4

5

6

7

8

9

10

11

12

14

13

V - 1

1

2

3

4

5

6

V - 2

Reference TCD

Helium

S/SL Injector

front

Splitvent

INJECT MODE V-1 (+) V-2 (-)

FOREFLUSH

Scion Instruments

Scion Instruments Natgas C Analyzer +He/H

2

Channel Reference Manual Page: 15

Backflush position

EFC-24

rear

Helium

Gas sample IN

Gas sample OUT

(To HeH2 channel)

Sample loop 250 µL

TCD

DEFC-13

middle

SCION-1

SC30128

Molsieve 13X

SC15919

Empty Delay column

SC15922

Hayesep P

SC15920

Vent 1

Liquid sample IN

Liquid sample OUT

EFC-25

front

Helium

EFC-24

middle

Helium

V-4

P

C

S

W

S

LSV 5

C

P

1

2

3

4

5

6

7

8

9

10

11

12

14

13

V - 1

1

2

3

4

5

6

V - 2

Reference TCD

Helium

S/SL Injector

front

Splitvent

BACKFLUSH MODE V-1 (-) V-2 (+)

BACKFLUSH

FID

DEFC-11

rear

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