Analysis of sulfonated naphthalene-formaldehyde condensates by ion-pair chromatography and their quantitative determination from aqueous environmental samples.
Analysis of sulfonated naphthalene-formaldehyde condensates by ion-pair chromatography and their quantitative determination from aqueous environmental samples.
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通过离子对色谱法分析磺化萘甲醛缩合物及其对水环境样品的定量测定。
DOI：
10.1021/ac000337j
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发表时间：
2000
影响因子：
7.4
通讯作者：
M. Jekel
中科院分区：
文献类型：
--
作者：
C. Wolf;T. Storm;F. Lange;T. Reemtsma;H. Brauch;S. Eberle;M. Jekel
开发了离子对固相萃取 (IPE)、带有荧光检测的离子对色谱 (IPC) 程序，用于定量分析磺化萘甲醛缩合物 (SNFC)，其提供的 SNFC 的全分辨率高达 n = 5 的缩合度，部分分辨率高达 n = 15。液相色谱-电喷雾电离-质谱法证实 SNFC 按缩合顺序洗脱。荧光检测中的响应因子被证明是质量恒定的，从而使我们能够确定 SNFC 总量。通过这种 IPC 方法，可以测定这些用作合成鞣剂、混凝土增塑剂和分散剂的大批量生产化学品（每年千吨）的重均分子量和数均分子量。对于 n = 2 至 n = 7，IPE 在莱茵河水中的回收率为 73% 至 85%，在自来水中的回收率为 79% 至 93%，500 mL 水中单个同系物的检测限为 3-8 ng/L。 IPE-IPC 程序适用于二次工业废水、莱茵河水、河岸滤液和地下水样品的样品。在处理过的废水中检测到多达 n = 6 的 SNFC。总浓度范围从二级处理的 SNFC 生产废水中的 208 微克/L 到地下水中的 < 1.4 微克/L。这些初步分析表明，SNFC 低聚物在水生环境中广泛存在。
An ion-pair solid-phase extraction (IPE), ion-pair chromatography (IPC) procedure with fluorescence detection for the quantitative analysis of sulfonated naphthalene-formaldehyde condensates (SNFC) was developed, which provides full resolution of SNFC up to a degree of condensation n = 5 and partial resolution up to n = 15. Liquid chromatography-electrospray ionization-mass spectrometry confirmed that SNFC elute in the order of condensation. Response factors in fluorescence detection proved to be mass-constant, thereby allowing us to determine total SNFC amounts. With this IPC method, the weight- and the number-average molecular weights of these high-volume production chemicals (kiloton per annum), used as synthetic tanning agents, concrete plasticizers, and dispersants, can be determined. Recoveries in IPE range from 73 to 85% in river Rhine water and from 79 to 93% in tap water for n = 2 to n = 7 with limits of detection of 3-8 ng/L for individual homologues from 500 mL of water. The IPE-IPC procedure was applied to samples of secondary industrial effluents, river Rhine water, a river bank filtrate, and a groundwater sample. SNFC up to n = 6 were detected in the treated effluents. Total concentrations ranged from 208 micrograms/L in a secondary treated SNFC production effluent to < 1.4 micrograms/L in groundwater. These first analyses suggest a widespread occurrence of the lower oligomers of SNFC in the aquatic environment.