柱前衍生高效液相色譜法測定黏膠纖維中單質硫

摘 要： 為了建立柱前衍生高效液相色譜（High performance liquid chromatography，HPLC）測定黏膠纖維中微量單質硫的方法，通過二氯甲烷-甲醇混合溶劑超聲提取黏膠纖維中單質硫；硫提取液與三苯基膦衍生后，在波長223 nm下采用HPLC檢測三苯基膦硫衍生物，并換算成單質硫含量。結果表明：常溫下單質硫與三苯基膦反應迅速，衍生轉化率高；三苯基膦硫在1～50 mg/L的范圍內線性關系良好，相關系數為0.99984，單質硫的定量限為0.407 mg/kg，加標回收率為102.75%～108.57%，相對標準偏差為0.77%～2.35%。該方法用于黏膠纖維中微量單質硫的測定，靈敏度高、重復性好。

關鍵詞：單質硫；黏膠纖維；柱前衍生；高效液相色譜；三苯基膦硫

中圖分類號：TQ340.7

文獻標志碼：A

文章編號：1673-3851 （2025） 03-0198-07

引文格式：李沖，陳海相，郎巧文，等. 柱前衍生高效液相色譜法測定黏膠纖維中單質硫［J］. 浙江理工大學學報（自然科學），2025，53（2）：198-204.

Reference Format： LI Chong，CHEN Haixiang，LANG Qiaowen，et al. Determination of elemental sulfur in viscose fibers by high performance liquid chromatography with pre-column derivatization［J］. Journal of Zhejiang Sci-Tech University，2025，53（2）：198-204.

Determination of elemental sulfur in viscose fibers by high performance liquid chromatography with pre-column derivatization

LI Chong， CHEN Haixiang， LANG Qiaowen， FENG Min， WANG Dawei

（National Engineering Lab for Textile Fiber Materials and Processing Technology， Zhejiang Sci-Tech University， Hangzhou 310018， China）

Abstract：To establish a pre-column derivatization high performance liquid chromatography （HPLC） method for the determination of trace amounts of elemental sulfur in viscose fibers， the experiment was carried out by ultrasonic extraction of elemental sulfur from viscose fibers by dichloromethane-methanol mixed solvent， and after derivatization of the sulfur extracting solution with triphenylphosphine， the derivatized product triphenylphosphine sulfur was detected by HPLC at a wavelength of 223 nm， and the elemental sulfur content was converted. The results showed that elemental sulfur reacted rapidly with triphenylphosphine at room temperature， and the derivatization conversion was high. The triphenylphosphine sulfur had a good linear relationship in the 1～50 mg/L range with a linear correlation coefficient of 0.99984. The limit of quantification （LOQ） for the elemental sulfur was 0.407 mg/kg， and the spiked recoveries ranged from 102.75% to 108.57% with the relative standard deviation （RSD） ranging from 0.77% to 2.35%. This method is used for the determination of trace elemental sulfur in viscose fibers with high sensitivity and good reproducibility.

Key words：elemental sulfur; viscose fibers; pre-columnar derivative; high performance liquid chromatography; triphenylphosphine sulfur

0 引 言

黏膠纖維是再生纖維素纖維。它是以天然纖維素（漿粨）為原料，經堿化、老化、磺化等工序制成纖維素磺酸酯，再溶于稀堿液制成黏膠，經濕法紡絲而制成。黏膠纖維在制備過程中產生單質硫，經過水洗與脫硫工序后，仍有部分單質硫殘留在黏膠纖維上^［1］。殘留的單質硫不僅腐蝕機械設備，還使纖維泛黃發暗、發硬、脆化，降低纖維強力^［1-2］，因此，殘硫量是評定黏膠纖維等級的重要指標之一。

目前，主要參照標準FZ/T 50014—2008《纖維素化學纖維殘硫量測定方法 直接碘量法》測定殘硫量，該標準中的測定采用氧化還原滴定化學分析法。鑒于FZ/T 50014—2008標準中終點判斷主觀、操作繁瑣、靈敏度低，且方法……