SYNSPEC GC s ALPHA 115 and ALPHA 116

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Methane/TotalNonMethaneHydroCarbons

Operator manual

Version January 2010 Synspec b.v. De Deimten 1 9747 AV Groningen Nederland [email protected]

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Preface

The purpose of this manual is to guide the operator in operating the Alpha 115 and the Alpha 116.

Read this manual first before you start to work with this instrument.

Contact your service engineer or expert if you have questions about this instrument. Keep this manual to use it in daily practice.

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1. Introduction

Synspec Alpha is an on-line gas chromatograph for measuring hydrocarbons in ambient air on behalf of environment and industry.

The measuring principle is true gas chromatography and the equipment is designed for field work.

Synspec Alpha 115 and 116 are compact gas chromatographs for measuring Methane and sum of total non-methane hydrocarbons in ambient air.

Standard analyses time is 3 min (180 sec).

The difference between the Synspec Alpha 115 and the Synspec Alpha 116 is the size of the loop and thus the detection limit.

With packed column and FID detector the Alpha 115 can detect from to 0,1 ppm to 1000 ppm Methane and from 0,05 ppm to 100 ppm total non methane hydrocarbons.

The Alpha 116 has a minimum detection limit of 1 ppm for methane and 1 ppm for total non methane. The reproducibility of the results is 1% of F(ull) S(cale).

Both types have an internal calibration switch for a fully automated calibration with zero air and span gas.

All the connections to the GC are 1/8 inch Swagelock connectors.

The GC has an internal Pentium computer with hard disk for storage of measurement results and 6” colour touch screen. The computer runs on Windows XPe and has the Synspec Alpha software pre-installed.

The GC can be controlled by using the touch screen, via keyboard and mouse, or remotely via RS 232/ Ethernet/ modem.

The GC Alpha software has three user levels :

1. Operator level. For the operator who looks at the results of the measurements and can start a standard calibration.

2. Service level. For the technician to adapt the machine for simple adaptations like changing the calibration gas bottle and the conditions for calibration.

3. Expert level. For the distributor or expert to install the machine, adapt all the settings, adapt the machine and software, do maintenance and trouble shooting. In this setting the principle and functioning of the system can really be altered. Which is not possible in levels 1 and 2.

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1.1 Safety notice WARNING:

The instrument is to be used by trained personnel ONLY.

Always disconnect the gas and power supply before opening the instrument.

Beware of electrostatic shocks to the internal computer. Do not drop metal parts in it. Use appropriate tools for maintenance.

Please note that the following risks have to be considered when working with the instrument: • Hydrogen and air at a pressure between 0.5 and 5 bar will be connected to the instrument. Personnel must be trained in safety issues of gasses in general and these gases specifically before working with these gases.

• The instrument works with a 230Vac or 110 Vac power supply. NOTICE:

Inspect the instrument for transport damage upon receiving. If you see any damages please do not switch on the analyser.

In case of damage contact your supplier within 8 days after receiving the instrument. Do not move an instrument when the internal computer is working to avoid damage of a hard disk.

Copy data from hard disk on a regular base. Otherwise the data can be lost which is at your own risk.

If you have questions about running the instrument, please contact your local supplier or Synspec BV. (Tel. +31 50 526 6454, fax +31 50 525 6540, e-mail [email protected]). If you modify the analyser the warranty is void and correct measuring is no longer guaranteed.

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1.2 General requirements

1. The instrument has to be placed in an air-conditioned room for operating at a stable temperature .

2. A space of standard H(eight)U(nit) from the bottom and 1 standard HU from the top has to be kept free for ventilating the system. Do not forget to reserve a place for the keyboard and mouse, preferably a board on slides, which can be 10 to 50 cm below the GC.

3. Power demand : Standard 230 Vac, 200 VA.

4. Room temperature : Between 5 and 40 oC.

5. Relative humidity : Must be 20 – 95 %. 6. Gases

a. Zero air as carrier gas, for the FID and for a zero span check (See Fig. 1.1). The quality should be 5.0 (99,999% pure) dry and clean at a pressure of 2,5 bar (38 PSI) and if it is used as a zero span check it should also be free of methane. Because the GC normally use 150 ml/min a standard gas bottle of 10 liter at 200 bar will only last for around 5,5 days. Therefore we recommend a zeroair generator (Fig. 1.1a).

b. Hydrogen as fuel for the FID. Quality 5 (99,999% pure) at a pressure of 2,5 bar (38 PSI)

c. Span gas we normally use a bottle of 1-2 ppm methane and 200-300 ppb Propane in air and set the pressure at 1 bar.

Left on top of the GC, above the touch screen you find the pressure regulators (Fig. 1.1).

Fig. 1.1 Pressure regulators in the GC

Pressure settings for hydrogen, zero air for FID and zero air for carrier (left to right). All recommended settings are marked.

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Fig. 1.1a Zero air and hydrogen generator 7. Gas couplings

All couplings to the instrument must be made in 1/8” Swagelok-compatible, for the gas supply in bronze, for the sample in stainless steel.

8. Pressure regulators (See Fig. 1.2). These must be of gaschromatographical quality. That means that they must be dust free and may not absorb or emit hydrocarbons. For air this is at least a nickel-plated bronze regulator with steel membrane, for bottles with maximal pressure 200 bar, range of the regulator 0 - 4 or 0 - 10 bar. For calibrating gases a stainless steel regulator with high quality steel membrane is preferred.

Fig. 1.2 Stainless steel regulator

9. Dust filter for sample lines : Material : Teflon filter membrane of 5 micron. Alternatively disposable nylon filters with glass frit or Teflon filters can be used.

10. Sample tubing :Clean inert tubing from PTFE (Teflon), FEP or stainless steel, even for short connecting pieces. Do not use the same tubing for taking ambient air samples and calibration samples. Use two tubing systems, that are only connected 5-15 cm before the sampling port.

Approval : CE approval for EMC conformity : EN 61010-1, EN 61000-6-2 and NEN 60111-6-3.

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1.3 What’s in the box

Fig. 1.3 Synspec Alpha 115

• 19″_{-keyboard + mouse + extension cables + touch screen pen}

• Power cable

• Memory stick (USB) • UTP cross cable

• Toolset and connectors (green) • Documents : manual, AED α_-list.

• Restriction

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1.4 Synspec Alpha 115 at a glance Visual appearance and connections

Fig. 1.4 Front

1. LCD-touch screen

2. 2 USB ports 3. Error indication LED 4. Idle/Running indication LED 5. Power switch Fig. 1.5 Rear 1. Mains 230 Vac/ 50 Hz Fuse 2A 2. Digital in/output 3. Analogue output 4. Analogue input 5. Pump out 6. Carrier gas inlet

7. Sample inlet 8. Spangas inlet 9. Zero Air inlet 10. Hydrogen inlet 11. Com 1 12. VGA (monitor) 13. LAN (local area network) 14. 2 USB 2.0 ports 15. Kb./MS (keyboard/mouse)

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Fig. 1.6 Connector overview

For adaption with a restriction, see extended calibration, description of the options. 1.5 Software

The alpha software is pre-installed on the GC and runs under windows XP embedded ( XPe). All the program settings are already installed and checked in our laboratory. Therefore the normal time to install the GC is minimal when all the requirements as described on par. 1.2 are met. The software is user friendly and has three levels: operator level, service level and expert level.

1.6 Hardware

• Internal computer with all the required software to run this GC

• Hard disk to store the program, measurement data and all the chromatograms

• LCD touch screen to see the results of the measurements, the status of the equipment and to move through the programs

1.7 Communication

With the GC Alpha there are several ways to communicate with the GC

• Digital out en inputs. The GC Alpha has seven digital output ports, and 4 digital inputs. These are freely programmable and can be used for the linking up of external equipment (external integrator or calibrator) or to react to external signals, like a remote start or a pressure switch.

• Analogue outputs and inputs. The GC Alpha has 4 analogue outputs to send a signal to an external datalogger. The Alpha also has 4 analogue inputs to use the computer of the GC alpha as a simple datalogger.

• USB. The GC Alpha has two USB connections at the front and two at the rear. These can be used for copying data or to attach external computer accessories.

• RS232. The GC Alpha has two comports that can be used for a RS232 connection. Over the RS232 data can be transmitted to a datalogger.

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• Ethernet connection. By using the Ethernet connection the software can be controlled from everywhere in the network, if the GC Alpha is attached to the internet the

machine can even be controlled over the internet, by using programs like team viewer, PC-anywhere and gotomyPC.

Data transfer Status information Instrument control Analogue

outputs Concentration values will be transmitted

No no

Analogue inputs

Can be used to read in data from other instruments

no no

Digital outputs

no Yes, all set

parameters in the digital communication protocol will be transmitted. Limited: some actions, like runstart, or start calibration can be set.

RS-232-communication Concentration values will be transmitted

Yes, all set parameters in the communication protocol will be transmitted. Limited: some actions, like runstart, or start calibration can be set. RS-232 modem, internet or ethernet (programs:PC Anywhere, VNC viewer and team viewer have been tested)

Yes, all data can be copied. Speed depends on modem and phone line, internet or Ethernet connection

Yes, as the GC screen can be seen

Full software control possible

USB connection

Can be used to copy data from the hard disk to zip drive, memory stick, CD-writeable etc.

no no

• Relay. The GC alpha has one relay which can be used for example to switch on an alarm signal when a certain concentration is reached.

1.7.1 Data handling

• The result of each measurement is stored in an monthly overview file and can be sent to a datalogger by using the analogue or over RS232.

• All the raw data (original chromatograms) are stored on the hard disk. In this way measurements can be checked and if the settings were not correct you can change it and the raw data (chromatograms) can be reprocessed.

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The GC Alpha is adapted for use as early-warning system for toxic compounds. Levels for low and high alarm can be set. Alarms can be given over modem, or over digital outputs. The GC can also be provided with a buzzer or lamp for an alarm on site.

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2. Operating Principle of the ALPHA 115

The measurements are based upon a TRUE GAS CHROMATOGRAPHIC

SEPARATION. This is done to avoid problems with catalytic functioning as often occurs with systems without the GC column resulting in inaccurate measurements.

Because it is a real gas chromatograph it contains a a loop ( to collect a sample), a compact oven ( to heat up the column), a column (to separate methane from total non-methane hydrocarbons) and an FID ( Flame Ionisation Detector).

Fig. 2.1 FID

Fig. 2.2 Drawing of FID principle

Principle: In a flame, oxygen and hydrogen are burned. When in a hydrogen flame other molecules pass, these will burn also and increase the amount of ions.

The ions generated by the flame are attracted to the positive side of an electrical field in the detector cell. The electrical current in the detector cell changes, this change is measured and has a direct correlation with the concentration.

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For our way of measuring we use a 10-port valve to switch between the different phases of the cycle. The use of a 10-port valve is mandatory for the principle of our measurements. A single measurement can be split into three different phases:

2.1 Collecting the sample

Fig. 2.3 Phase one, the sample loop is filled

The sample is pulled by an internal sample pump from the “sample in” through the “sample loop” to the “sample out” collecting a volume of sample that is equal to the volume inside of the “ sample loop”. Than 10-port valve switches to reach phase 2.

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2.2 Analysing of methane

Fig. 2.4 Phase two, detection and analysing of methane

The carrier gas carries the volume of sample from the sample loop to the column and to the FID. The column retains the TNMHC and the methane is passing through the column. So in this phase only the methane is detected. For the burning of the FID the hydrogen and the zero air also flow to the detector. To go phase 3 the 10-port valve is again switched.

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2.3 Analysing of total non methane hydrocarbons

Fig. 2.5 Phase 3, detection and analysing of total non methane hydrocarbons (TNMHC)

The flow of carrier gas over the column is now, in the opposite direction ( backflush) in comparison to phase 2, going to the FID. GC columns normally separate the different hydrocarbons, by using the backflush principle we regroup these different hydrocarbons resulting in only one peak for the TNMHC. If Phase 3 is compared with phase 1 it is clear that both phases can be run at the same time. Meaning that a sample can be collected while the TNMHC is being analysed. This saves time and results in shorter cycle times, thus more measurements per time unit.

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3. For the operator

When all connectors are connected the right way and the GC is started, then you will see the the actual data screen, see next picture (Fig. 3.1) :

3.1 Actual data

Fig. 3.1 Actual data (operator level)

For a better explanation in this manual numbers in red are placed on the screen picture. 3.1.1 Language and help

Actual data item 1 (Fig. 3.1) ITEMS : Above this number you see the name of this screen thus you are now looking at the GCAlpha-Actual data screen. The items “Language” and “Help” are not activated yet.

The language is English and for help after you have read this manual thoroughly, you can call your service engineer or expert.

3.1.2 Actual value

Actual data item 2 (Fig. 3.1) ACTUAL VALUE : Here you see the Actual value for CH4 (methane) i.e.

15727.7 v-ppb (volume-parts per billion)

Below this you see the Actual value of TNMHC (TotalNonMethaneHydroCarbons) i.e. 550.1 v-ppb.

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Actual data item 3 (Fig. 3.1) TREND : Below “Trend” you see a little picture of a graph made of measurement values from the last 50 measurements of CH4. By clicking on this little picture you get

Fig. 3.2 i.e. : the last 50 measurement data of methane (CH4). Under “Actual value” you read the value 15727.7 v-ppb, this is the last measured value. On the trend list is this the value number 1 produced on 4/12-14.41. The other values have older dates and so number 50 have the oldest measurement date. On this list you also see the average value of the 50

measurement values i.e. 17828.25 v-ppb.

With the same principle as for CH4, below the little picture of the “CH4-graph” you see of a graph made of measurement values from the last 50 measurements of TNMHC.

By clicking on this little picture you get Fig. 3.3 i.e. the last 50 measurement data of TNMHC. The Actual value of 550.13 v-ppb is the last measured value. On the trend list is this the value number 1 produced on the same date 4/12-14.41.. The average value of TNMHC is here 277.77 v-ppb.

Fig. 3.2 last 50 measurementsdata of CH4 Fig. 3.3 Last 50 measurementsdata of TNMHC

So when after this you make again a measurement, the values of this measurement will be the last measured values and will be placed as the new number 1 on the trend list. The previous number 1 on the list with the values 15727.7 v-ppb for CH4 and 550.13 v-ppb for TNMHC are then placed on number 2 on the trend list and so on. The former number 50 on the list disappears and former number 49 on the list is now the new number 50.

Of course the Average values will change also.

When you click on “OK” on both of the trend lists you get back to the Actual data screen. 3.1.4 Status

Actual data item 4 (Fig. 3.1) STATUS : At the “Status” you can see what the GC is busy with at this moment. On the screen you read “Running Analizing”, this means that the GC now is busy with analyzing. Other possible “Status” messages on screen are : “Running waiting to start” (The waiting time between 2 runs), “Running injecting” (The GC is busy with sample injection), “Power up check" (The GC is checking the power) and “Error” (Something wrong is happened before, during or after a run).

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3.1.5 Recalibrate

Actual data item 5 (Fig. 3.1) RECALIBRATE : After clicking on “Recalibrate”, you are going to start a (Re)calibration. The status message of calibration is changed in “Waiting to start”. If you do want to start a (re)calibration, please check first if the sample tubing is attached to the spangas inlet. There are 3 possibilities that you are going to see as status message of calibration : a. Waiting to start, b. Running and c. Idle.

c. Idle, means out of specifications or either the deviation from the last one is too large, or that the values of the repetitions are too much different.

3.1.6 Calibration trend

Actual data item 6 (Fig. 3.1) CALIBRATION TREND : By clicking on the surface with number 6, calibration trend,you get the calibration trend for methane (Fig. 3.4) and on this trend you see 2 radiobuttons, one for CH4 (methane) which is tapped and one for TNMHC and by tapping the “TNMHC” button you get the TNMHC trend (Fig.3.5).

Fig. 3.4 calibration trend of CH4 Fig. 3.5 calibration trend of TNMHC

Fig. 3.6 calibration trend of CH4 not yet done Fig. 3.7 calibration trend of TNMHC not yet done The trend learns us to see how stable the calibration is. The lesser the graph goes up and down the more stable the calibration is. But when you see one straight line in the middle, this means that there is no calibration yet (Figures 3.6 and 3.7).

The graph is a good help to follow the calibration in sensitivity and or stability. By clicking on close you return to the Actual data screen.

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Actual data item 7 (Fig. 3.1) VIEW ALARM LOG : By clicking on View alarm log, you get an overview of the history of all the alarms (Fig. 3.8)

By scrolling with the mouse you will find the last given alarm at the end of the list. On the Actual data screen (Fig. 3.1) the status message of the system alarm shows “No error”, this means nothing is going wrong.

Fig. 3.8 Dialog 3.1.8 Restart FID

Actual data item 8 (Fig. 3.1) RESTART FID : By clicking on this, The FID will start automatically. The FID detector in Actual data shows if the FID is running properly. The temperature normally should be between 80 and 150 oC. :

On the Actual data screen (Fig. 3.1) the status message of the detector is “OK, temperature 99”. This means the flame is burning and detector temperature is 99 _°C and thus OK. 3.1.9 Chromatogram

Actual data item 9 (Fig. 3.1) CHROMATOGRAM : By clicking on “Chromatogram” the Datafile screen appears, and then you click on “Options” and you see Fig. 3.9. On this screen you will see the chromatogram, the graph with the peaks of CH4 and TNMHC when you load a datafile.

All datafiles, measurement, calibration - and validation files are saved in directories. These directories are joined in a structure, the GC Alpha directory structure (Fig. 3.18).

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See “datafile item 6” how to load a datafile after you have clicked on “Load datafile”.

3.2 Datafile

Fig. 3.9 Datafile (operator level)

Datafile item 1 (Fig. 3.9) : Here we have 3 items, Options, Language and Help. The Options are :

3.2.1 SELECT VIEW ITEMS :

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The way of setting for additional info on the chromatogram happens by clicking in the empty square(s) next to the item concerns and then by clicking OK. Here you see that

“Oventemperature” and “pump” are marked. By clicking on “Chromatogram” (See Fig. 3.1) again you will see Fig. 3.11. The green tube with a blue square in it shows the functioning of the pump and the red irregular running line presents the oventemperature.

Other options are not applicable or activated. Click “Cancel” means you don’t want to change anything and go back to the previous screen.

“OK” and “Cancel” are not mentioned again in this manual.

Fig. 3.11 red line is “oventemperature”, the blue square is “the pump”. 3.2.2 SELECT SCREEN ELEMENTS :

Click on “Select screen elements” and you get Fig. 3.12.

Fig. 3.12 Select screen elements Fig. 3.13 Datafile with all screen elements With select screen elements you can choose to see :

On Fig. 3.12 all the screen elements are marked and these elements you can see on the chromatogram on Fig. 3.13.

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1. Peak windows : This is a window set over the peak to make sure the whole chromatogram is integrated and also important for setting retention time lock. The setting method for this is for the expert.

2. Retention time : The time from injecting to showing a peak. This should be always (almost) the same.

3. Integration values : An integration value is the surface area of a peak, important for determining the concentration of the compound.

4. Calculated peakheights : Important for the integration of the chromatogram. 5. Horizontal axis seconds : With this you set the chromatogram scale in seconds. 3.2.3 ADJUST DETECTOR Y-AXIS OFFSET :

Click on “Adjust detector Y-axis offset”, the next screen appears.

Fig. 3.14 Y-axis offset adjust

With Y-axis offset adjust you can set the axis higher in case the baseline “disappears” below the chromatogram scale.

Sometimes you see a chromatogram “disappears” with baseline under zero. This you can correct by adjusting the Y-axis offset, choosing a fit value in the block next to “FID Detector” (Fig. 3.14).

3.2.4 Attenuation :

Datafile item 2 (Fig. 3.9) : In Figures 3.9 and 3.14a in close-up you see how the

chromatogram can be attenuated. Click on Previous, you see the previous value, click on Next you see the next value.

When the peak is very small you can make it bigger, but the rest of the peaks becomes also bigger. For example :

To attenuate the chromatogram to 10x, click on 1 and then on 10 and so on.

The attenuating of the chromatogram has totally no influence on the measurement results. Standard setting is 4x10 (See Fig. 3.15). Other setting is shown on Fig. 3.16.

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Fig. 3.15 att. 4x10 Fig. 3.16 att. 4x1 3.2.5 Chromatogram scale, date and cycle time :

Datafile item 3 (Fig. 3.9) : This is the chromatogram scale where above the chromatogram shows.

Fig. 3.17 detail from fig. 3.9

Datafile item 4 (Fig. 3.9) : In Fig. 3.9 and Fig. 3.17 in detail the left you see a little box with the value 0, this is where you read the minutes and seconds of the scale. When you set the scale in 10% the total minutes/seconds is 10_′ 00_′′and so on. Next to this you see a little scale in blue/grey from 0 to more than 30. By clicking in this part you can look at the

chromatogram further on the scale. When you click at the end of the scale the red vertical line moves to the end and the scale moves to the end to 60 at 100%. At the last part you can set the scale in 100%, 50%, 25% and 10% of the scale by clicking on the value you want .

Datafile item 5 (Fig. 3.9) : Here you see the date, time and cycle time (Fig. 3.9). 3.2.6 Load datafile :

Datafile item 6 (Fig. 3.9) : Click on the datafile screen on “Load datafile” to load a datafile of a measurement, calibration or validation (Fig. 3.9). To choose the file you want, you have to follow the directory structure (See Fig. 3.18).

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Fig. 3.18 Directory structure GCALPHA 115

Datafile is used to recall files, data files (D), calibration files (C) or validation files (V). Choose the directory for the correct month (for instance D_0903 for March 2009).

The chromatograms are saved in month-directories, with day-subdirectories, with a filename derived from the measurement time in days, hours, minutes, prefixed by a m: m_281435.bin. The chromatogram appears if you double-click a file. The scale in the x and the y-axis is the same as in the chromatogram that is being measured.

The rundat.txt file (RDyymm.TXT) down below Fig. 3.18 and Fig. 3.19 is a summary of all measurements per month with many information like date, time, concentration and integration value (Area).

Fig. 3.19 rundat.txt file

Explanation of the rundat.txt file (Fig. 3.19) :

1. Code N : Normal data or data from normal measurements. Code V : Validation data or data from validation measurements. Code C : Calibration data or data from calibration measurements. 2. Date : Date of measuring.

3. Time : Time of measuring. 4. Sample 1

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6. Conc-1 : Concentration of methane (CH4) in v-ppb 7. Reti-1 : Retention time of CH4.

8. Conc-2 : Concentration of total non methane hydrocarbons (TNMHC) in v-ppb. 9. Area-2 : Integration value of TNMHC.

10. Reti-2 : Retention time of TNMHC.

You can move freely between the modes actual data and load datafile.

Actual data item 10 (Fig. 3.1) CLOSE : To close the program (Fig. 3.1).

Actual data item 11 (Fig. 3.1) LOGIN : The Login for the service level and the expert level (only for the technician and distributor).

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Index

1 10-port valve · 13, 14, 15, 16 A Actual data · 17, 18, 19, 20, 27 Actual value · 17, 18

ADJUST DETECTOR Y-AXIS OFFSET · 23 AED α_{-list · 7} ambient air · 3, 7 Analog inputs · 10 Analog outputs · 10 B

bronze · See_{gas couplings}

C Calculated peakheights · 23 calibration · 3, 7, 9, 10, 19, 20, 24, 26 CALIBRATION TREND · 19 Carrier gas · 9 Chromatogram · 20, 22 D Datafile · 20, 21, 22, 23, 24, 26 digital in- and/or output ports · 10 Digital outputs · 10 E early-warning system · 11 F FEP · 7 filter membrane · 7 G Gas couplings · 6 glass frit · 7 H Help · 17, 21

Horizontal axis seconds · 23

I integration value · 23, 26 Integration values · 23 ITEMS · 17, 21 L Language · 17, 21 low and high alarm · 11 M

methane · 3, 5, 13, 14, 15, 16, 17, 18, 19, 27

N

nickel-plated bronze regulator · 6 O Options · 20, 21 Oventemperature · 22 P Peak windows · 23 Pressure regulators · 6

Pressure regulators in the GC · 6 PTFE (Teflon) · 7

R

RESTART FID · 20 Retention time · 23, 27

RS-232 modem and PC Anywhere · 10 RS-232-communication · 10

S

sample · 6, 7, 13, 14, 15, 16, 18, 19 Sample tubing · 7

SELECT SCREEN ELEMENTS · 22 software license · 7

stainless steel · 7, See gas couplings

stainless steel regulator · 6 status message · 19, 20 Swagelok-compatible · 6

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T Teflon · 7 toxic compounds · 11 U USB connection · 11 V

VIEW ALARM LOG · 20 W

warranty · 4 Z