SN/T 2763.6-2014Chemical analysis of nickel laterite ore - Part 6: Determination of nickel, calcium, titanium, magnesium, copper, cobalt, chromium, zinc and phosphorus content - Inductively coupled plasma atomic emission spectrometric method (English PDF)
红土镍矿化学分析方法 第6部分：镍、钙、钛、锰、铜、铬、锌、磷含量的测定 电感耦合等离子体原子发射光谱法
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Issued by
General Administration of Quality Supervision, Inspection and Quarantine of PRC
Level / Type
National · Recommended
Issue date
December 12, 2012
Implementation date
July 1, 2013
Scope
SN/T 2763.6-2014 is the English-translated version of 红土镍矿化学分析方法 第6部分：镍、钙、钛、锰、铜、铬、锌、磷含量的测定 电感耦合等离子体原子发射光谱法.
SN/T 2763.6-2014 is the Chinese standard "Chemical analysis of nickel laterite ore - Part 6: Determination of nickel, calcium, titanium, magnesium, copper, cobalt, chromium, zinc and phosphorus content - Inductively coupled plasma atomic emission spectrometric method".
Its scope clause reads: This standard specifies a gas chromatographic method for determining the free glycerol content in crude glycerol. This standard applies to crude glycerol, which are byproducts of biodiesel production with a mass fraction of less than 95%, industrial-grade saponified glycerol, and synthetic glycerol.
Its clauses include method summary; reagents; apparatus; sample; analysis steps; result calculation and representation. It was issued by the General Administration of Quality Supervision, Inspection and Quarantine of PRC on 2012-12-12 and took effect on 2013-07-01.
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Document preview — SN/T 2763.6-2014
National Standard of the People's Republic of China
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of PRC
Contents
- Foreword...3
- 1 Scope...4
- 2 Method summary...4
- 3 Reagents...4
- 4 Apparatus...4
- 5 Sample...5
- 6 Analysis steps...5
- 7 Result calculation and representation...5
- 8 Precision...7
- Appendix A (Informative) Chromatographic conditions...8
- Appendix B (Informative) Typical chromatogram...9
1 Scope
This standard specifies a gas chromatographic method for determining the free glycerol content in crude glycerol.
This standard applies to crude glycerol, which are byproducts of biodiesel production with a mass fraction of less than 95%, industrial-grade saponified glycerol, and synthetic glycerol.
2 Method summary
After acetic anhydride is added, the sample is heated, and a derivatization reaction is carried out to generate glycerin triacetate, which is then determined by using a gas chromatograph and quantified using the internal standard method.
3 Reagents
Unless otherwise specified, only reagents confirmed to be of analytical grade shall be used in the analysis.
3.1 Glycerol standard (C3H8O3). with a content of greater than 99%.
3.2 Acetic anhydride (C4H6O3). with a content of greater than 95%.
3.3 Internal standard. ethyl benzoate (C9H10O2), with a content of greater than 99%.
4 Apparatus
4.1 Gas chromatograph. It is equipped with a flame ionization detector (FID).
4.2 Microsyringe. 10 µL.
4.3 Pipettes. 1 mL, 25 mL.
4.4 Dropping bottle. 25 mL.
4.5 Stoppered conical flask. 125 mL.
4.6 Analytical balance. with a sensitivity of 0.1 mg.
5 Sample
The crude glycerol sample is thoroughly mixed and placed in a dropping bottle for later use.
6 Analysis steps
6.1 Sample preparation
Weigh 0.4 g~0.5 g of the above crude glycerol sample into a stoppered conical flask using the differential weighing method, accurate to 0.2 mg.
6.2 Derivatization
Add 25 mL of acetic anhydride (3.2) to a stoppered conical flask containing the glycerol sample, and place it in a 120 °C oven to react for 2 h. Remove and cool to room temperature.
6.3 Chromatographic conditions
See Appendix A.
6.4 Preparation of standard solutions
Weigh 0.1 g, 0.2 g, 0.3 g, 0.4 g, and 0.5 g of glycerol standard (3.1) into stoppered conical flasks using the differential weighing method, accurate to 0.2 mg, and derivatize them together with the sample according to 6.2.
6.5 Measurement
Take the derivatized sample solution (6.2) and standard solution (6.4), accurately transfer 1 mL of ethyl benzoate (3.3) into an Erlenmeyer flask, shake well, take the supernatant, and proceed with the conditions as described in 6.3.See Appendix B for the gas chromatogram of the glycerol derivative.
6.6 Blank test
Perform a blank test on acetic anhydride according to the above determination steps.
7 Result calculation and representation
7.1 Plotting the standard curve
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 9 pages — is available in the English PDF.
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Related Standards
SN/T 2763.1-2011 — Determination of multi-components in nickel laterite ores. Part 1: X-ray fluores cence spectrometric method
SN/T 2763.3-2012 — Chemical analysis of nickel laterite ore - Part 3: Determination of total iron content - Titanium (III) chloride reduction methods
SN/T 2763.4-2012 — Chemical analysis of nickel laterite ore - Part 4: Determination of nickel, cobalt, aluminum, magnesium and phosphorus content - Inductively coupled plasma atomic emission spectrometric method
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