EN 14110 Methanol content by HS

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   |description = Determination of Methanol content by Headspace
   |description = Determination of Methanol content by Headspace
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=== Overview ===
=== Overview ===
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Glycerin content can indicate the quality of biodiesel. Glycerin can be in the form of free glycerin or bound glycerin in the form of glycerides. Total glycerin is the sum of these.  A high content of free and total glycerin can lead to buildup in fuel tanks, clogged fuel systems, injector fouling and valve deposits. Unrelated glycerides and free glycerin make the product behave more like soap rather than fuel.
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EN14110 describes the required method for methanol determination in biodiesel.
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A high methanol content can raise vapor pressure and increase flammability in biodiesel.
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ASTM Method D6571 specifications serve as the benchmark which identifies the standards that pure biodiesel (B100) must meet before being used as a fuel or blended with petrodiesel. There are 14 different required tests according to ASTM D6751-03. The US National Biodiesel Board has adopted the ASTM biodiesel specification and analytical methodology.  ASTM recommends test method D6584 for the analysis of glycerin in biodiesel fuel by gas chromatography.
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Gas chromatography can also serve as a tool for process troubleshooting during biodiesel production to ensure trouble-free operation of the fuel in diesel engines. Monitoring the level of free glycerin and any unrelated mono-, di-, and triglycerides will indicate the efficiency and progress of the chemical reaction during the process of making biodiesel.
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ASTM Method D6584 provides for the quantitative determination of free and total glycerin in B-100 methyl esters by gas chromatography. The range of detection for free glycerin is 0.005 to 0.05 mass%, and total glycerin from 0.05 to 0.5 mass %. This method is not applicable to vegetable oil methyl esters obtained from lauric oils, such as coconut oil and palmkernel oil.
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=== Significant Markets  ===
=== Significant Markets  ===
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* Fleet Managers
* Fleet Managers
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'''ASTM Method D684'''
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'''EN Method 14110'''
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'''9. Calibration and Standardization'''
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EN 14110: Fat and oil derivatives – Fatty Acid Methyl Esters (FAME) - Determination of methanol content
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'''9.2 Standard Solutions''' – Prepare the five standard solutions in ''Table 3'' by transferring the specified volumes by means of Microliter syringes to 10mL septa vials. Add to each of the five standard solutions 100uL of MSTFA. Close the vial and shake. Allow the vial to stand for 15 to 20 minutes at room temperature. Add approximately 8 mL n-Heptane to vial and shake.
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Biodiesel can consist of different fatty acid methyl esters, depending on the oils used during production. For the determination of methanol in such a complex matrix, gas chromatography in combination with headspace injection is the recommended method. This enables separation of low-boiling methanol from the high-boiling fatty acid methyl esters already during the sample preparation step.
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The biodiesel samples are heated in a gas-tight 20 mL vial. Methanol is a low-boiling point compound and is enriched in the gas-phase while the high-boiling point compounds remain in the liquid phase. After a specific time, equilibrium is reached and a constant volume can be sampled from the gas-phase (headspace) of the vial and injected into the GC system.
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|+ '''TABLE 3 Standard Solutions'''
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! Standard Solution Number !! 1 !!  2 !!  3 !!  4 !!  5
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! uL of glycerin stock solution
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| 10 || 30 || 50 || 70 || 100
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! uL of monoolein stock solution
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| 20 || 50 || 100 || 150 || 200
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! uL of diolein stock solution
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| 10 || 20 || 40 || 70 || 100
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! uL of triolein stock solution
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| 10 || 20 || 40 || 70 || 100
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! uL of butanetriol stock solution
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| 100 || 100 || 100 || 100 || 100
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! uL of tricaprin stock solution
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| 100 || 100 || 100 || 100 || 100
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|}
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'''9.4 Standardization'''<br/> 
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GC Run time is approximately 10 minutes
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'''9.5''' Inject 1 uL of the reaction mixture into the cool-on-column injection port and start the analysis.
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'''10. Procedure'''<br/>
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=== Photos ===
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'''10.1''' Weigh to the nearest 0.1 mg approximately 100 mg of sample directly into a 10 mL septa vial. Using Microliter syringes, add exactly 100 uL of each internal standard and MSTFA. Shake the vials, and allow to set for 15 to 20 minutes at room temperature. Add approximately 8 mL of n-Heptane to vial and shake.
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[[Image:HP6890.jpg|200px|thumb|left|Representative System shown with Agilent 7890 and Combi PAL]] <br><br><br><br><br><br><br>
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'''10.2''' Inject 1 uL of the reaction mixture into the cool on-column injection port and start the analysis.
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=== LEAP's Approach ===
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[[Image:6584.jpg|200px|thumb|left|System shown with Agilent 7890 and Twin PAL]]
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The Lower PAL is the Prep PAL and runs on Cycle Composer Software. All of the sample prep is performed with this PAL. There is a 100ul syringe for the solvent transfers. There are (7) 2mL solvent locations. There is a DISPTool that is hooked up to a 5 mL dilutor syringe for the 8 mL Heptane addition. There is a fast wash station that Wash1 is filled with Toluene and Wash 2 is filled with Heptane. There is an agitator that is set at 35 deg C and 500RPM to do the mixing.
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The Upper PAL is the Inject PAL and runs under ChemStation Software control. This requires Agilent CTC Control Software supplied by Agilent. It is using a 5 ul syringe with a tapered needle to do 1 ul on column injections into the rear injection port. There is a fast wash station that Wash1 is filled with Toluene and Wash 2 is filled with Heptane.
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The expected Sample Prep Time is approximately 26 minutes<br/>
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The expected GC Runtime is approximately 31.81 minutes<br/>
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The expected GC Cool down time is approximately 7 minutes<br/>
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<br/><br/>
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=== Software Control ===
=== Software Control ===
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The Lower PAL is the Prep PAL and runs on Cycle Composer Software.  
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Currently the [http://www.leapwiki.com/mediawiki/index.php?title=Category:Combi COMBI  ] [http://leapwiki.com/mediawiki/index.php?title=Category:PAL     PAL] and runs on via the hand held due to the desire for look ahead functionality.
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The Upper PAL is the Inject PAL and runs under ChemStation Software control.
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The incubation time is 45 minutes and the GC runtime is approximately 10 minutes
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Can also be run under Cycle Composer or Agilent CTC control software without look ahead functionality.
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<br/> <br/> <br/> <br/> <br/> <br/> <br/><br/><br/>
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== Screenshots ==
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=== Screenshots ===
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<gallery>
<gallery>
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   Image:5stndardsprep.png  | Cycle Composer 5 Standards Prep
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   Image:hs1.png  | Cycle Composer method parameters
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  Image:6584SamplePrepISMSTFA.png | Cycle Composer Sample Prep
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  Image:CCSTD prep sample list.png  | Cycle Composer Prep Standards
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  Image:6584StandardsPrep.png | ChemStation Sequence Table
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  Image:SequencetableA.png | ChemStation Sequence Table
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  Image:1_ul_inj.png | ChemStation PAL Method for Injection
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  Image:GCInjfor6584.png | ChemStation and Cycle for injection
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</gallery>
</gallery>
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== Video ==
 
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*[[:Image:DISPTool.ppt | Dispense Tool movement]]
 
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== Useful links ==
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===Useful links ===
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[[Image:Www icon.png|40px]] [http://www.4cleanfuels.com/biofuels/BioDQuality8-07/FQ_workshop-PiedmontBioFuels.pdf An overview of all tests that must be run by Piedmont Biofuels]
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[[Image:Www icon.png|40px]] [http://www.chem.agilent.com/cag/prod/GC/Biodiesel_QR.pdf A good general reference site by Agilent]
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Biodieselanalytical.com  A good general reference site on Biodiesel automation theory and practice [http://biodieselanalytical.com/instsum.aspx]
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[[Image:Www icon.png|40px]] [http://biodiesel.engr.uconn.edu/home/Stuart.pdf UCONN.com  A good general reference site on Biodiesel ASTM Methods]
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A good general reference site by Agilent [http://www.chem.agilent.com/cag/prod/GC/Biodiesel_QR.pdf]
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[[Image:Www icon.png|40px]] [http://www.biodiesel.orgwww.biodiesel.org  A good general reference site on Biodiesel  ]
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UCONN.com  A good general reference site on Biodiesel without buying the ASTM Methods [http://biodiesel.engr.uconn.edu/home/Stuart.pdf]
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[[Image:Www icon.png|40px]] [http://www.biodieselmagazine.com/plant-list.jsp Biodiesel Plant Listing ]
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Biodiesel Plant Listing [http://www.biodieselmagazine.com/plant-list.jsp]
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[[Image:Www icon.png|40px]] [http://www.biodieselconference.org/2009/default.asp Biodiesel Conference 2009 ]
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Biodiesel Conference 2009 [http://www.biodieselconference.org/2009/default.asp]
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=== Videos of PAL ===
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<br>
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[[Image:Movie Icon.png|40px]]
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[http://www.youtube.com/user/LEAPTechnologies#g/u LEAP's PAL Application Videos on YouTube]
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<br>
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== Publications ==
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----
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*[[:Image:ASTM_D6584_Free_&_Total_Glycerin.pdf‎ | ASTM D6584 - not for redistribution]]
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{{logo}}
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== Other Reference material ==
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LEAP provides automated workstation instrumentation solutions based on the LEAP CTC PAL X, Y, Z syringe only autosampler robot from LEAP Technologies. This extremely flexible, precise, and adaptable liquid handling robotic platform is available in a variety of lengths and options depending on the requirements of your sample preparation and injections for your UHPLC, LC or GC chromatography.LEAP offers full support and service for the PAL platform in addition to being able to write custom macros, cycles, and scheduling to your applications. Please contact LEAP Technologies on how we can help you get maximized throughput with flexible pipetting automation solutions.
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*[[:Image:LEAP_ASTM_D_6584_Quick_User_Guide_Rev_5.pdf‎  | ASTM D6584 - Quick User Guide]]
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=== Contact LEAP ===
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{{contact|topic=LEAP and the PAL Platform}}
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[[Category: Biofuel]]
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[[Category:Application_Solutions]]
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[[Category:Cycle Composer]]
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[[Category:Gas Chromatography]]
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[[Category:Chronos]]

Current revision

Biofuels
Application Type
  Sample Inject
Application ID
  Biodiesel EN14110
Description
  Determination of Methanol content by Headspace
 ↳ leaptec.com  ↳ leapwiki.com
 ↳ leaptec.com
 ↳ leapwiki.com

Contents

Overview

EN14110 describes the required method for methanol determination in biodiesel. A high methanol content can raise vapor pressure and increase flammability in biodiesel.

Significant Markets

  • Biodiesel Manufactures
  • Biodiesel Blenders
  • Biodiesel Distributors
  • Biofuels CROs
  • Fleet Managers

EN Method 14110

EN 14110: Fat and oil derivatives – Fatty Acid Methyl Esters (FAME) - Determination of methanol content

Biodiesel can consist of different fatty acid methyl esters, depending on the oils used during production. For the determination of methanol in such a complex matrix, gas chromatography in combination with headspace injection is the recommended method. This enables separation of low-boiling methanol from the high-boiling fatty acid methyl esters already during the sample preparation step.

The biodiesel samples are heated in a gas-tight 20 mL vial. Methanol is a low-boiling point compound and is enriched in the gas-phase while the high-boiling point compounds remain in the liquid phase. After a specific time, equilibrium is reached and a constant volume can be sampled from the gas-phase (headspace) of the vial and injected into the GC system.

GC Run time is approximately 10 minutes

Photos

Representative System shown with Agilent 7890 and Combi PAL
Representative System shown with Agilent 7890 and Combi PAL







Software Control

Currently the COMBI PAL and runs on via the hand held due to the desire for look ahead functionality.

The incubation time is 45 minutes and the GC runtime is approximately 10 minutes

Can also be run under Cycle Composer or Agilent CTC control software without look ahead functionality.








Screenshots

Cycle Composer method parameters


Useful links

An overview of all tests that must be run by Piedmont Biofuels

A good general reference site by Agilent

UCONN.com A good general reference site on Biodiesel ASTM Methods

A good general reference site on Biodiesel

Biodiesel Plant Listing

Biodiesel Conference 2009

Videos of PAL


LEAP's PAL Application Videos on YouTube

 ↳ leaptec.com  ↳ leapwiki.com
 ↳ leaptec.com
 ↳ leapwiki.com

LEAP provides automated workstation instrumentation solutions based on the LEAP CTC PAL X, Y, Z syringe only autosampler robot from LEAP Technologies. This extremely flexible, precise, and adaptable liquid handling robotic platform is available in a variety of lengths and options depending on the requirements of your sample preparation and injections for your UHPLC, LC or GC chromatography.LEAP offers full support and service for the PAL platform in addition to being able to write custom macros, cycles, and scheduling to your applications. Please contact LEAP Technologies on how we can help you get maximized throughput with flexible pipetting automation solutions.

Contact LEAP

Contact LEAP

For additional information about LEAP and the PAL Platform, please contact LEAP Technologies.

Retrieved from "http://leapwiki.com/mediawiki/index.php/EN_14110_Methanol_content_by_HS"
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