EN 14110 Methanol content by HS

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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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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'''
'''9. Calibration and Standardization'''
'''9. Calibration and Standardization'''
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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.
'''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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{| border="1"
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=== Photos ===
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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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[[Image:HP6890.jpg|200px|thumb|left|Representative System shown with Agilent 7890 and Combi PAL]]
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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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'''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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'''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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=== Software Control ===
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The expected GC Runtime is approximately 31.81 minutes<br/>
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Currently the COMBI PAL and runs on via the hand held due to the desire for look ahead funcationality.
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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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Can also be run uncer Cycle Coposer or Agilent CTC cotrol software without look ahead fuctionality.
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=== Software Control ===
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The Lower PAL is the Prep PAL and runs on Cycle Composer Software.  
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The Upper PAL is the Inject PAL and runs under ChemStation Software control.
 
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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
   Image:6584SamplePrepISMSTFA.png | Cycle Composer Sample Prep
   Image:6584SamplePrepISMSTFA.png | Cycle Composer Sample Prep
   Image:CCSTD prep sample list.png  | Cycle Composer Prep Standards
   Image:CCSTD prep sample list.png  | Cycle Composer Prep Standards

Revision as of 14:44, 9 February 2009

Biofuels
Application Type
  Sample Inject
Application ID
  Biodiesel EN14110
Description
  Determination of Methanol content by Headspace

Contents

Overview

EN14110 describes the required method for methanol determination in biodiesel.

Significant Markets

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

EN Method 14110

9. Calibration and Standardization

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.

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 funcationality.

Can also be run uncer Cycle Coposer or Agilent CTC cotrol software without look ahead fuctionality.


Screenshots

Cycle Composer method parameters

Cycle Composer Sample Prep

Cycle Composer Prep Standards

ChemStation Sequence Table

ChemStation Sequence Table

ChemStation PAL Method for Injection

ChemStation and Cycle for injection

Video

Useful links

Biodieselanalytical.com A good general reference site on Biodiesel automation theory and practice [1]

A good general reference site by Agilent [2]

UCONN.com A good general reference site on Biodiesel without buying the ASTM Methods [3]

Biodiesel Plant Listing [4]

Biodiesel Conference 2009 [5]

Publications

Other Reference material

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