首页 馆藏资源 舆情信息 标准服务 科研活动 关于我们
现行 ASTM D7742-17(2024)
到馆提醒
收藏跟踪
购买正版
Standard Practice for Determination of Nonylphenol Polyethoxylates (NPnEO, 3 ≤ n ≤ 18) and Octylphenol Polyethoxylates (OPnEO, 2 ≤ n ≤ 12) in Water by Single Reaction Monitoring (SRM) Liquid Chromatography/ Tandem Mass Spectrometry (LC/MS/MS) 用单一反应监测(SRM)液相色谱/串联质谱法(LC/MS/MS)测定水中壬基酚多乙氧基化物(NPnEO 3≤n≤18)和辛基酚多甲氧基化品(OPnEO 2≤n≤12)的标准实施规程
发布日期: 2024-04-01
1.1 本规程涵盖壬基酚聚氧乙烯醚(NPnEO,3 ≤ n ≤ 18) 和辛基苯酚聚乙氧基酯(OPnEO,2 ≤ n ≤ 12) 通过使用直接注射液相色谱法(LC)的单反应监测(SRM)液相色谱/串联质谱法(LC/MS/MS)在水中进行检测,并通过串联质谱法检测。这是一种具有合格定量数据的筛选方法,用于检查水样中是否存在长链乙氧基化物。 1.1.1 所有数据都是合格的,因为没有每种烷基酚乙氧基化物(APEO)的纯标准品,并且这些纯标准品的合成和表征将非常昂贵。Igepal 2. 使用品牌标准,其中含有各种链长的烷基酚乙氧基化物(APEOs)的混合物。假设仪器在最佳电喷雾电离锥下的响应和每个APEO的碰撞电压相同,则在内部对混合物进行表征。这一假设可能不准确,用于确定标准中每种乙氧基化物的合格量。正壬基酚二乙氧基化物(n-NP2EO)替代品可作为纯表征标准品获得,因此,未估计该浓度和回收率数据。APEO不受美国环保局的监管,但壬基酚是NPnEO的分解产物,受淡水和盐水排放者的监管。 污水处理厂(STP)要求通过ASTM提供这一做法,以筛选进入STP的APEO来源的进水或出水。利益在于阻止较长链APEO的来源进入STP,以满足污水处理指南。基于以上内容,这是一种实践而非测试方法。使用这种做法可以对样品进行比较,以确定哪种样品的APEO浓度更高。 1.2 单位-- 以国际单位制表示的数值应视为标准。本规程不包括其他计量单位。 1.3 中显示的估计筛选范围 表1 根据表4中所示的1级和7级校准标准品的浓度计算。 如第节所述,这些数字是合格的 1. ,并且必须如实报告。 图1- 5. 显示了每种分析物在1级浓度下的SRM色谱图以及信噪比(S/N)。这是一种筛选实践,没有给出方法检测限值。1级浓度下每种分析物的S/N比必须至少为5:1,以获得足够的灵敏度。如果仪器不能满足标准,则必须将筛选限值提高到可接受的水平。 图1 SRM色谱图NP3EO-NP8EO 图2 SRM色谱图NP9EO-NP14EO 图3 SRM色谱图NP15EO-NP18EO和n-NP2EO 图4 SRM色谱图OP2EO-OP7EO 图5 SRM色谱图OP8EO-OP12EO 1. 4. 本标准并不旨在解决与其使用相关的所有安全问题(如有)。本标准的使用者有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 1.5 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ====意义和用途====== 5.1 这种做法是为了支持美国政府而制定的。 美国环保局水资源办公室,芝加哥地区实验室(CRL)的科学技术办公室。 5.2 壬基酚(NP)和辛基酚(OP)已被证明对水生生物具有毒性作用。NP和OP的主要来源是来自常见的商业表面活性剂,它们是长链APEO。最广泛使用的表面活性剂是壬基酚聚乙氧基酯(NPnEO),其平均乙氧基化物链长为9。APEO易于生物降解,形成NP1EO、NP2EO、壬基酚羧酸盐(NPEC)和NP。NP也会生物降解,但可能以微量水平直接释放到环境水中。本规程筛选较长链的APEO,这些APEO可能以较高的水平进入STP,并可能导致STP违反壬基酚的允许排放浓度。
1.1 This practice covers the determination of nonylphenol polyethoxylates (NPnEO, 3 ≤ n ≤ 18) and octylphenol polyethoxylates (OPnEO, 2 ≤ n ≤ 12) in water by Single Reaction Monitoring (SRM) Liquid Chromatography/ Tandem Mass Spectrometry (LC/MS/MS) using direct injection liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS) detection. This is a screening practice with qualified quantitative data to check for the presence of longer chain ethoxylates in a water sample. 1.1.1 All data are qualified because neat standards of each alkylphenol ethoxylate (APEO) are not available and the synthesis and characterization of these neat standards would be very expensive. The Igepal 2 brand standards, which contain a mixture of various chain lengths of the alkylphenol ethoxylates (APEOs), were used. The mixture was characterized in-house assuming the instrument response at an optimum electrospray ionization cone and collision voltage for each APEO was the same. This assumption, which may not be accurate, is used to determine qualified amounts of each ethoxylate in the standards. The n-Nonylphenol diethoxylate (n-NP2EO) surrogate was available as a neat characterized standard, therefore, this concentration and recovery data was not estimated. APEOs are not regulated by the EPA, but nonylphenol, a breakdown product of NPnEOs, is regulated for fresh and saltwater dischargers. A request by a sewage treatment plant (STP) was made to make this practice available through ASTM in order to screen for the influent or effluent from sources of APEOs coming into the STP. The interest lies in stopping the source of the longer chain APEOs from entering the STP in order to meet effluent guidelines. Based upon the above, this is a practice rather than a test method. A comparison between samples is possible using this practice to determine which has a higher concentration of APEOs. 1.2 Units— The values stated in SI units are to be regarded as standard. No other units of measurement are included in this practice. 1.3 The estimated screening range shown in Table 1 was calculated from the concentration of the Level 1 and 7 calibration standards shown in Table 4. These numbers are qualified, as explained in Section 1 , and must be reported as such. Figs. 1- 5 show the SRM chromatograms of each analyte at the Level 1 concentration with the signal to noise (S/N) ratio. This is a screening practice and method detection limits are not given. The S/N ratio for each analyte at the Level 1 concentration must be at least 5:1 for adequate sensitivity. If the instrument can not meet the criteria, the screening limit must be raised to an acceptable level. FIG. 1 SRM Chromatograms NP3EO-NP8EO FIG. 2 SRM Chromatograms NP9EO-NP14EO FIG. 3 SRM Chromatograms NP15EO-NP18EO and n-NP2EO FIG. 4 SRM Chromatograms OP2EO-OP7EO FIG. 5 SRM Chromatograms OP8EO-OP12EO 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 5.1 This practice has been developed in support of the U.S. EPA Office of Water, Office of Science and Technology by the Chicago Regional Laboratory (CRL). 5.2 Nonylphenol (NP) and Octylphenol (OP) have been shown to have toxic effects in aquatic organisms. The prominent source of NP and OP is from common commercial surfactants which are longer chain APEOs. The most widely used surfactant is nonylphenol polyethoxylate (NPnEO) which has an average ethoxylate chain length of nine. The APEOs are readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This practice screens for the longer chain APEOs which may enter the STP at elevated levels and may cause a STP to violate its permitted discharge concentration of nonylphenol.
分类信息
关联关系
研制信息
归口单位: D19.06
相似标准/计划/法规