GB/T 40323-2021 in English
VALIDDetermination of octamethylcyclotetrasiloxane(D4), decamethylcyclopentasiloxane(D5) and dodecamethylcyclohexasiloxane(D6) in textile dyeing and finishing auxiliaries
- Issued on:2021-08-20
- Implemented on:2022-03-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$214.00
《GB/T 40323-2021纺织染整助剂产品中八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)和十二甲基环六硅氧烷(D6)的测定》由TC134(全国染料标准化技术委员会)归口,TC134SC1(全国染料标准化技术委员会印染助剂分会)执行,主管部门为中国石油和化学工业联合会。
Introduction
Standard background and scope of application
This standard is formulated to meet the detection needs of three types of cyclic siloxanes (D4, D5, D6) in textile dyeing and finishing auxiliaries. The detection limits of these two methods are both 50mg/kg, filling the gap in the detection standards for organosilicon pollutants in my country's textile chemicals.
Comparison of core detection methods
| Technical parameters | Gas chromatography (GC) method | Static headspace-gas chromatography (HS-GC) method |
|---|---|---|
| Pretreatment time | About 15min | 30min equilibrium time |
| Standard solution concentration | 1000mg/L high concentration stock solution | 10000mg/L high concentration stock solution |
| Recovery rate range | 92.5%-101.1% | 90.0%-101.1% |
| Applicable sample types | Conventional liquid additives | High volatility/viscous samples |
Key operating points
Acetic acid suppression technology
Both methods use acetic acid isopropanol solution (1:9) as a stabilizer, which can effectively inhibit the decomposition of siloxane during the detection process. The GC method requires the addition of 1.0mL of this solution to both the standard working solution and the sample solution.
Optimization of Chromatographic Conditions
It is recommended to use a HP-5 chromatographic column (30m×320μm×0.25μm), and adopt a programmed temperature rise: 50℃ for 3min, then increase to 250℃ at 10℃/min and hold for 8min. The FID detector temperature needs to be maintained at 300℃.
Technology Evolution Analysis
Compared with the traditional extraction method, the static headspace technology introduced in this standard has three major advantages: ① avoid sample matrix interference; ② reduce organic solvent consumption; ③ high degree of automation. However, it should be noted that the 180℃ equilibrium temperature may affect thermally unstable samples.
Implementation recommendations
- GC method is preferred for samples with D4 content >1000mg/kg
- Regularly verify the linearity of the standard curve (R²≥0.995)
- Strictly control the shelf life of the standard solution under 4℃ storage conditions
- The characteristic ion abundance deviation requirements must be met during mass spectrometry confirmation (see Table C.1)

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