Safety
To demonstrate is sensitivity, some performance tests have been done. Analysis of 8 Sulphur compounds from external certifi ed standards have been done. Below are shown the results obtained for the stability tests and linearity tests after 20 consecutive analysis performed on the following components:
All tests performed are part of a protocol document pertaining to analyser validation and are defi ned by a European third part laboratory. To validate the instrument, it is required to perform 20 analysis and to get the results in compliance with ISO 5725-2. The samples are generated from different standards.
Hydrogen sulphide
Methyl Mercaptan (MM or MTM) Ethyl Mercaptan (EM or ETM) Dimethyl Sulphide (DMS)
(iso) 2-Propyl Mercaptan (IPM) ter Butyl Mercaptan (TBM) (N) 1-Propyl Mercaptan (NPM) TetraHydroThiophene (THT)
Table 1: List of molecules analysed during the test
Table 2 here above summarise the different results obtained per compound. Concentration (mg/m3
)
Mean SD
Relative Error (%) Repeatability (%)
Reference concentration
H2S MM EM IPM TBM THT DMS STD 3,16
9,06
0,011 1,50 0,72 3,11
(+/-4%) Table 2: Concentrations obtained for H2 6,02
0,21 2,38 6,01
8,05
2,06 1,20 8,22
5,18
0,96 1,21 5,13
27,20
0,031 0,072 0,048 0,031 0,146 0,84 0,68 9,14
0,51 1,07
(+/-4%) (+/-4%) (+/-4%) (+/-4%)
27,06 (+/-4%)
6,04
0,021 0,19 0,71 6,03
(+/-10%) S, MM, EM, IPM, TBM, THT and DMS STD over 20 measurements
Table 3 represents the criteria for compliance with ISO 19739 norm and the obtained values using the energyMEDOR®
instrument. Repeatability (%)
Performance criteria
H2 S
MTM (or MM) ETM (or EM) IPM
TBM THT
3 2 4
10 7 4
Obtained value 0,72
0,68 2,38 1,20 1,21 1,07
Relative reproducibility (%)
Performance criteria
25 10 30 20 25 20
Obtained value 1,50
0,84 0,21 2,06 0,96 0,51
Table 3: Comparison between performance criteria in compliance with ISO 19739 and obtained values.
The relative reproducibility and repeatability values are much better than performance criteria values as defi ned in the ISO 19739 norm. All tested compounds have a linear response (to SSD) in the trial conditions (i.e. range of 0 – 5 mg/m3
for most of sulphur compounds and THT range 0-25 mg/m3
with a R2 > 0.995 for all compounds. So the conclusion was that the performance criteria are in compliance with the norm.
An example of a chromatogram obtained with the energyMEDOR® around 1mg/m3
is shown in Figure 1 below. for the measurement of H2 S at ) Conclusion
There is a clear global tendency for analysing Sulphur compounds with speciation in the oil and gas fi eld but also on other markets, with a demand under expansion in industries like shale gas, Biogas, odour and CO2
in beverage. This should remain important in coming years.
Certifi cations are also a key issue for the company as it is important to continue to invest in these processes to validate the technologies for specifi c fi elds and applications. Chromatotec® Ex d applications and sampling module development allow to extend the scope of its MEDOR®
evolution.
investments in solution.
The diversifi cations of the processes and the need for effi ciency improvements result in customers looking for customised and performant solutions. These specifi c needs are at the base of Chromatotec®
Chromatotec® ’s energyMEDOR® appears to be the best alternative for these applications since it only
needs a small amount of nitrogen or zero air to operate its Sulphur Specifi c Detector. This certifi ed solution has been designed to operate in zone I and II and can be used with 230V, 115V and 24V power supply making it quite unique on such type of market.
Author Contact Details Figure 1: Typical chromatogram obtained with energyMEDOR
Franck Amiet – president and CEO & Jean-Philippe Amiet – M. Sc. Export Project Manager Mickaël Gezat – Project Manager, Chromatotec • 15 rue d’artiguelongue, Saint-Antoine, 33240 Val de Virvée France • Tel: +33 (0)5 57 94 06 26 • Email:
info@chromatotec.com • Web:
www.chromatotec.com
Figure 2: Analysis of H2 S, TOS and TS in two minutes H2 S CH3-SH
CH3CH2-SH CH3-S-CH3
(CH3)2-CH-SH (CH3)3-C-SH
CH3CH2CH2-SH C4H8S
At the end of each chromatogram, a validation of results is done by injecting and analysing the DMS from the internal calibration device (permeation tube).
Another application for natural gas market is related to the Integrity Monitoring. During the extraction of raw natural gas and following processing, Midstream companies are required to track the level of H2
S and TS (Total Sulphur = H2 S +
Total Organic Sulphur (TOS)). If the concentration measured exceed the required levels, the Midstream companies must shut down the gathering line until the measurement are showing the required concentration levels again.
S from the other sulphur species (shown in Figure 2).
For these analysis, the sample is fi rst loaded into a loop and then injected in an analytical column to separate H2
To expand the applications of the MEDOR® CHROMATOTEC®
, a specifi c sampling module has been developed by to inject extremely low volume (from 0.1 to 1 µL) into the autoGC. LPG analysis
(Propane and butane), which is directly connected in the sampling module inlet. Then it is vaporised and injected into the MEDOR®
thanks to the very low volume injected the MEDOR®
directly. Another application is for high concentration up to low %: instrument is not disturbed.
Other applications for heavier liquid hydrocarbon like condensate or gasoline are also available; as soon as they can be vaporised in the heated sampling module it is possible to analyse them with MEDOR®
.
53
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