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Determination of Free and Total Glycerin in B-100 Biodiesel by ASTM D6584 and EN 14105
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Biodiesel fuel must conform to ASTM D6751 specifications for use in
diesel engines. Testing for this confirmation is outlined in ASTM D6584
and similar method DIN EN 14105. These methods provide for the quantitative
determination of free and total glycerin in 100% biodiesel fuel (B100
methyl esters) by high temperature gas chromatography after silylating
the sample with N-methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA).
Biodiesel Calibration Standards
Derivatization Reagents
GC Analysis
Accessories – Vials and Syringes |
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Supelco glycerin impurities in biodiesel reference solutions meet the specifications
called out in ASTM D6584 and DIN EN 14105. Our reference solutions have been carefully formulated
to save 4–6 hours in prep time, minimize the possibility of human error,
and eliminate the need to prepare pyridine dilutions. Our standards
offer:
- raw materials tested for identity and purity
- stock solutions for preparing your own multi-component solutions
- multilevel, multi-component solutions ready for derivatization
- monoglyceride commercial mixture for EN14105
- internal standard solutions
- certificate of composition shipped with each standard
- instructions for derivatization with each kit
Our standards are manufactured under the Quality Management System which is
registered under ISO 9001:2000.
Ordering Information for Calibration Standards and Standard Solutions
| Description |
Cat. No. |
| ASTM D6584 |
| Glycerin, 1 mL, 500 µg/mL in pyridine |
44892-U |
| Monoolein, 3 mL, 5000 µg/mL in pyridine |
44893-U |
| Diolein solution, 2 mL, 5000 µg/mL in pyridine
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44894-U |
| Triolein, 2 mL, 5000 µg/mL in pyridine |
44895-U |
| Butanetriol Internal Standard #1, 5 mL, 1000 µg/mL
in pyridine |
44896-U |
| Tricaprin Internal Standard #2, 5 mL, 8000 µg/mL
in pyridine |
44897-U |
| ASTM D6584 Individual Stock and Internal Standards Mix
Kit |
44898-U |
| ASTM D6584 Standard Solution 1, 1 mL, in pyridine (varied) |
44899-U |
| ASTM D6584 Standard Solution 2, 1 mL, in pyridine (varied) |
44914-U |
| ASTM D6584 Standard Solution 3, 1 mL, in pyridine (varied) |
44915-U |
| ASTM D6584 Standard Solution 4, 1 mL, in pyridine (varied) |
44916-U |
| ASTM D6584 Standard Solution 5, 1 mL, in pyridine (varied) |
44917-U |
| ASTM D6584 Individual Standard Solution & Internal
Standards Kit |
44918-U |
| DIN EN 14105 |
| EN 14105:2003 Monoglyceride Stock Solution, 1 mL, 10 mg/mL in pyridine |
49446-U |
| EN 14105:2003 Standard Solution 1, 1 mL, in pyridine (varied) |
49441-U |
| EN 14105:2003 Standard Solution 2, 1 mL, in pyridine (varied) |
49442-U |
| EN 14105:2003 Standard Solution 3, 1 mL, in pyridine (varied) |
49443-U |
| EN 14105:2003 Standard Solution 4, 1 mL, in pyridine (varied) |
49444-U |
| EN 14105:2003 Standard Solution Kit |
49445-U |
MSTFA (N-methyl-N-(trimethylsilyl)trifluoroacetamide) is cited in DIN EN
14105 and ASTM D6584 for silylating the free and total glycerides of B-100 biodiesel prior
to analysis by gas chromatography. MSTFA transforms the glycerides into a thermally
stabile, but volatile, derivative for measuring glycerin impurities in biodiesel.
MSTFA is sensitive to moisture. We recommend purchasing the smallest quantity
possible for your application, and storing the material in a desiccator at a
temperature between 4-8 ºC
Ordering Information for MSTFA reagent
| Description |
Cat. No. |
| N-Methyl-N-(trimethylsilyl)trifluoroacetamide (derivatization
grade) |
394866 |
HT-5 fused silica capillary GC columns are designed for high temperature analyses
– up to 480ºC in temperature-programmed applications. The high temperature
capability of this column makes it well suited for the analysis of glyceride
and triglyceride esters following the chromatographic analysis conditions cited
in ASTM D6584.
View a chromatogram of biodiesel MSFTA-derivatives, obtained on a HT-5 capillary
GC column.
The use of a guard column with the HT-5 column will protect it from excess
reagent and non-volatile compounds, extending the column life.
Ordering Information for GC Columns and Connectors
| Description |
Cat. No. |
| Capillary GC column, HT-5, length x I.D. 12 m x 0.32
mm, df 0.10 µm |
25002 |
| Capillary GC column, HT-5, length x I.D. 6 m x 0.53 mm,
df 0.10 µm |
25004 |
Supeltex® M-2B Double-Tapered Ferrule
I.D. 0.5/0.8 mm, 0.32 mm I.D. to 0.53 mm I.D. Column, pack of 2 |
22586 |
| Capillary Column Butt Connector - body only (ferrules
not included) |
23804 |
| Replacement Capillary Column nuts , 1/16 in. male finger-tight
(knurled) |
23812 |
Supelco offers a large selection of vials and
syringes for most applications.
Listed below are the vials and syringes recommended for use with Supelco brand
biodiesel standards when following ASTM D6584 methodology.
Ordering Information for Vials
| Description |
Cat. No. |
| Vials, screw top with phenolic hole cap, pre-assembled,
15 mL, amber glass |
27014-U |
| Vials, screw top with phenolic hole cap, pre-assembled,
15 mL, clear glass |
27158 |
| Vials, screw top, amber glass (cap not included), 15
mL, amber glass, thread 18-400, O.D. × height 21 mm × 70 mm |
27088-U |
| Vials, screw top, graduated (vial only), 15 mL, clear
glass (with graduations), thread 18-400, O.D. × height 21 mm ×
70 mm |
27026 |
| Screw cap with hole, for use with 15 mL vial (with 18
mm thread), black phenolic cap |
27165 |
| Septa, PTFE/red rubber, for use with 15 mL vial, PTFE/red
rubber, diam. × thickness 16 mm × 0.060 in. |
27167 |
Ordering Information for Syringes
| Description |
Cat. No. |
Hamilton® syringe, cemented needle, pt.#5
volume 100 µL, needle size 22s ga (cone tip, side-port) |
24535 |
Hamilton® syringe, 700 series, cemented needle
volume 100 µL, needle size 22s ga (bevel tip) |
20737 |
Hamilton® syringe, cemented needle, pt.#5
volume 250 µL, needle size 22s ga (cone tip, side-port) |
24536 |
Hamilton® syringe, 700 series, cemented needle
volume 250 µL, needle size 22s ga (bevel tip) |
20738 |
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