重金屬混存物感應耦合電漿∕原子發散光譜（ICP/AES）同步分析方法驗證

The Evaluation of Simultaneous Determination of Heavy Metals in Fumes by Inductively Coupled Plasma / Atomic Emission Spectrometry (ICP/AES)

本研究係配合行政院勞工委員會勞工安全衛生研究所標準檢測方法的建立需求，建立作業環境空氣中重金屬混存物感應耦合電漿／原子發散光譜(ICP/AES)同步分析方法，以有效提高檢測效能，達到經濟、快速及準確分析之目的。本研究所要驗證的元素共有 20 個，研究並針對 1)樣品前處理及儀器操作條件建立；2)檢量線範圍、檢量線品管及方法偵測極限；3)採樣及分析干擾；4)回收率評估；5)分析變異係數；6)樣品儲存穩定性測試及7)真實樣品分析等項目進行探討。研究結果顯示 ICP/AES 之線性範圍皆非常寬廣(102 ~104 )；品管樣品分析的結果亦符合驗証程序所規定≦10.0%的要求；方法偵測極限，則隨不同元素有所差異，約在0.001 µg/mL (Be)~0.31 µg/mL (Se) 之間；回收率及分析變異係數(CVa)亦符合所規定回收率≧75%及分析變異係數≦7%之要求。至於樣品儲存穩定性測試結果顯示，無論是室溫遮光保存及冷藏保存，在 28 天內其相對測試值均在 90%~110% 範圍內。為了評估方法的實用性，本研究特別針對焊接作業所產生之金屬燻煙進行真實樣品的採樣與分析，結果顯示有部分作業環境的氧化鐵及錳的排放值已超過容許濃度標準(PEL)，證明本方法對於真實作業環境樣品之檢測具有可行性。

This research follows the requirement of the Institute of Occupational Safety and Health (IOSH) of the Council of Labor Affairs of Executive Yuan (CLAEY) and completes the standard analysis method. “The Establishment of the Simultaneous Determination of Heavy Metals in Working Environments by Inductively Coupled Plasma/Atomic Emission Spectrometry (ICP/AES)”, which can increase the efficiency of the analysis and meet economical, fast and accurate purposes. This research contains the validation of 20 elements and include the study of the following items: 1) the pretreatment of the samples and the establishment of the instrument operating conditions; 2) the calibration curve range, the quality control of the calibration curve and the method detection limit (MDL); 3) the interference of sampling and analysis; 4) the evaluation of recovery; 5) analysis coefficient of variation (CVa); 6) the stability test for the storage of samples; and 7) the real sample analysis. The results show that there are wide linear ranges (102 ~ 104) for the 20 elements under the validation method by ICP/AES. The standard deviations for the quality control samples meet the validation requirement of ≦10.0%; As for the method detection limit (MDL) , the values of MDL for the elements are about between 0.001 μg/mL (for Be)~0.31 μg/mL (for Se) . In the aspect of recovery and analysis coefficient of variation (CVa) , both meet the validation requirements of ≧75% and ≦7% respectively. For the stability test for the storage of samples, the test values are between 90%~110% for both the lightprotected storage at room temperature and cold preservation within 28 days. In order to evaluate this method in actual practice, this research conducts the sampling and analysis for the real samples of the metal fumes during the soldering operation, and the data show that the emission values of ferric oxide and manganese are over the permissible exposure limits (PELs) for certain working environment, and this proves that this standard analysis method is suitable for workplace sample analysis.