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SN/T 3344-2012: Determination of free glycerin in crude glycerin. Gas chromatography
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SN/T 3344-2012: Determination of free glycerin in crude glycerin. Gas chromatography

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Determination of free glycerin in crude glycerin.Gas chromatography People's Republic of China Entry-Exit Inspection and Quarantine Standards Crude glycerol free glycerol determination Gas chromatography Issued on. 2012-12-12 2013-07-01 implementation People's Republic of China The State Administration of Quality Supervision, Inspection and Quarantine released

Foreword

This standard was drafted in accordance with GB/T 1.1-2009 given rules. This standard is proposed and managed by the National Certification and Accreditation Administration Committee. This standard was drafted. People's Republic of China Jiangsu Entry-Exit Inspection and Quarantine Bureau. The main drafters of this standard. Ding Hua, Li Xidong, Zhouqiu Hong, lord Hing. Crude glycerol free glycerol determination Gas chromatography

1 Scope

This standard specifies the gas chromatographic method crude glycerol free glycerol content. This standard applies to the mass fraction of less than 95% of the by-product bio-diesel made crude glycerin, industrial saponification glycerol synthetic glycerine.

2 Method summary

After the sample was added acetic anhydride was heated to produce triacetin after derivatization reaction was measured by gas chromatography internal standard method.

3 Reagents

Unless otherwise indicated in the analysis using only recognized as analytical reagents. Sample Glycerin 3.1 (C3H8O3). content of more than 99%. Acetic anhydride 3.2 (C4H6O3). content greater than 95%. 3.3 Internal standard. ethyl benzoate (C9H10O2), content greater than 99%.

4 Instrument

4.1 Gas chromatograph. equipped with a flame ionization detector (FID). 4.2 micro-injector. 10μL. 4.3 Pipette. 1mL, 25mL. 4.4 dropper. 25mL. 4.5 stoppered conical flask. 125mL. 4.6 Analysis of balance. a sense of the amount of 0.1mg.

5 Sample

Crude glycerin samples were thoroughly mixed, placed in a dropper bottle and set aside. Step 6 Analysis 6.1 Preparation of the sample By Difference Method Weigh 0.4g ~ 0.5g sample of the crude glycerol in stoppered Erlenmeyer flask, accurate to 0.2mg. 6.2 Derivative In a sample containing glycerin stoppered Erlenmeyer flask, 25mL acetic anhydride (3.2), placed in an oven at 120 ℃ reaction 2h. Remove to cooling ...