SH/T 1613.2-2018 in English
VALIDPetroleum o-xylene- Part 2:Determination of purity and hydrocarbon impurities- Gas chromatography
- Issued on:2018-04-30
- Implemented on:2018-09-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$165.00
本标准规定了用气相色谱法测定石油邻二甲苯的纯度及烃类杂质含量。
本标准适用于测定纯度不低于90.0%（质量分数）的石油邻二甲苯，本部分对于非芳烃、苯、甲苯、乙苯、间二甲苯、对二甲苯、异丙苯、正丙苯、苯乙烯、三甲苯、甲乙苯、对二乙苯等烃类杂质的检测范围为（0.001～3.5）% （质量分数）。
Introduction
Core changes in the standard revision
| Revision dimensions | 1995 edition | 2018 edition |
|---|---|---|
| Method principle | Internal standard method only | Newly added correction area normalization method |
| Chromatographic column | Packing column | Capillary column (60m×0.32mm×0.50μm) |
| Precision | Repeatability limit only | Added reproducibility limit requirements |
Key technical points
1. Comparison of detection principles
Internal standard method: By adding n-undecane as internal standard, the hydrogen flame ionization detector (FID) is used for detection, and the ratio of the impurity peak area to the internal standard peak area is calculated. It is suitable for absolute content determination.
Corrected area normalization method: Based on the effective carbon number theory, the response factors of each component are corrected and directly normalized. It needs to be verified with quality control samples and is suitable for rapid screening.
2. Key instrument parameters
Chromatographic column: Polyethylene glycol capillary column (PEG-20M), column temperature program: initial temperature 60℃→10℃/min→150℃ (5min)
Detector: FID temperature 300℃, carrier gas flow rate 1.0mL/min (He/N2), split ratio 100:1
Implementation suggestions
1. Method selection strategy
- Arbitration analysis: Internal standard method is preferred
- Process control: Correction area normalization method can be used, but it needs to be verified with quality control samples every day
2. Quality control requirements
| Indicators | Control standards |
|---|---|
| Correction factor RSD | ≤5% |
| Purity verification deviation | ≤0.05% (mass fraction) |
Solutions to typical problems
Problem 1: Poor separation of non-aromatic hydrocarbons and benzene→ It is recommended to adjust the initial column temperature to 50℃ or reduce the heating rate
Problem 2: Components above C10 are not eluted→ The termination temperature can be increased to 180℃ and the holding time can be extended
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