CAJ | 학술논문

应用电感耦合等离子体质谱法（ICP －MS）测定化探样品中的 Ag 时，两个同位素107 Ag 和109 Ag 分别受90 Zr16 O1 H、91 Zr16 O 和92 Zr16 O1 H、93 Nb16 O 等的干扰，即使采用干扰系数法校正，测定结果误差仍较大。本文采用硝酸－氢氟酸－高氯酸封闭分解样品，氨水沉淀分离干扰元素 Zr 后以103 Rh 为内标用 ICP －MS 测定，溶液中残留 Zr 对107 Ag 的测定干扰采用干扰系数法进行校正。方法检出限（3σ）为4．1 ng／g，相对标准偏差（n ＝12）为2．5％～7．8％。经53个地球化学标准物质验证，溶液中的 Ag 未见损失。本方法是在氨性介质中 Ag 与氨形成稳定的络合离子，而 Zr 则生成氢氧化物沉淀，实现了 Ag 和 Zr 的分离，大大减小了 Zr 对 Ag的测定干扰；采用封闭分解样品，减少用酸量，降低了样品空白值，操作方法比高压密闭分解和 P507萃淋树脂分离方法更简便快速。
응용전감우합등리자체질보법（ICP －MS）측정화탐양품중적 Ag 시，량개동위소107 Ag 화109 Ag 분별수90 Zr16 O1 H、91 Zr16 O 화92 Zr16 O1 H、93 Nb16 O 등적간우，즉사채용간우계수법교정，측정결과오차잉교대。본문채용초산－경불산－고록산봉폐분해양품，안수침정분리간우원소 Zr 후이103 Rh 위내표용 ICP －MS 측정，용액중잔류 Zr 대107 Ag 적측정간우채용간우계수법진행교정。방법검출한（3σ）위4．1 ng／g，상대표준편차（n ＝12）위2．5％～7．8％。경53개지구화학표준물질험증，용액중적 Ag 미견손실。본방법시재안성개질중 Ag 여안형성은정적락합리자，이 Zr 칙생성경양화물침정，실현료 Ag 화 Zr 적분리，대대감소료 Zr 대 Ag적측정간우；채용봉폐분해양품，감소용산량，강저료양품공백치，조작방법비고압밀폐분해화 P507췌림수지분리방법경간편쾌속。
Isobaric ions interfere with two isotopes of Ag during determination by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS),i.e.,90 Zr16 O1 H and 91 Zr16 O on 107 Ag,and 92 Zr16 O1 H and 93 Nb16 O on 109 Ag.Although an interference correction coefficient method was used for the calibration of the analytical results,the analytical errors remain serious.In the proposed method,samples were closed decomposed by nitric acid,hydrofluoric acid,and perchloric acid.Ammonia was used to precipitate Zr and the purified Ag was determined by ICP-MS using 103 Rh as the internal standard.The interference caused by the residual Zr was calibrated by the interference coefficient method.The method has a detection limit (3σ)of 4.1 ng/g and relative standard deviation (n =12)ranging from 2.5% to 7.8%.Determination of Ag in 53 primary certified materials of geochemical exploration indicates no loss of Ag.Using ammonium as the reagent,separation of Zr and Ag was successfully achieved due to the formation of the stable Ag-ammonium complex and Zr-hydroxide precipitate.The separation of Ag from Zr has reduced the interferences of Zr on Ag.Compared with the high-pressure sealed decomposition method and the P507 extraction resin separation method,the closed sample decomposition method is much simpler with less acid used and a lower blank.