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Why my Headspace does not separate the analyte from the sample?

Question asked by jvelasco on Mar 14, 2019
Latest reply on Aug 8, 2019 by james_jenkins

Hello everyone, I need your help.

 

Headspace does not separate the analyte from the sample

 

DGA test (analysis of combustible gases for transformer oil)

 

Configuration toga with headspace, method c astm 3612 (ref 2009)

 

Observations:

The sample is loaded into the headspace with the configurations suggested by the standard and stabilized for 30 minutes.

No type of combustible gas has been detected.

 

The calibration method is carried out with the patterns in the gas phase and the headspace and the chromatograph and the traceability in the results (whenever the sample is loaded in the gas phase, the compounds are detected).

 

Tests carried out to date (to deal with the subject of the sample)

Temperature change (up to 150 ° C)

Change of equilibrium time (20, 25 and 60 minutes)

Change of loop filling times, change of injection time, change of vial pressure, change of air and change of needles - currently installed nickel 232-2790010-ehs; Tests were performed with 301-220-HSP, with negative results related to an error in the rise engine)

 

Changes were made in the volume of the oil sample (5.10 and 15 ml), joints and unions were checked.

 

IMAGE 1 and 2: This is the standard graph

 

STD 100_001.jpg

STD 100_002.jpg

IMAGE 3 and 4: This is the oil test graph:

13 DE MARZO DE 2019_001.jpg

 

OTHER IMAGES: For reference.

WhatsApp Image 2019-03-14 at 9.50.25 AM.jpeg

WhatsApp Image 2019-03-14 at 9.50.35 AM.jpeg

WhatsApp Image 2019-03-14 at 9.50.57 AM.jpeg

WhatsApp Image 2019-03-14 at 9.53.30 AM.jpeg

WhatsApp Image 2019-03-14 at 9.56.19 AM.jpeg

WhatsApp Image 2019-03-14 at 9.56.34 AM.jpeg

 

Attached video.

 

Thank you.

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