岩矿测试
巖礦測試
암광측시
ROCK AND MINERAL ANALYSIS
2015年
4期
459-463
,共5页
地球化学样品%铂%钯%野外分析%巯基棉富集%分光光度法
地毬化學樣品%鉑%鈀%野外分析%巰基棉富集%分光光度法
지구화학양품%박%파%야외분석%구기면부집%분광광도법
geo-chemical samples%platinum%palladium%field analysis%sulfhydryl cotton preconcentraction%Spectrophotometry
对于地球化学样品中铂钯的测定，传统和现代分析方法均是建立在试金或树脂及活性炭富集后用分光光度法或电感耦合等离子体质谱法测定，而在野外满足不了这些条件。本文基于样品的性质及分光光度法的适应性强等特点，开发了一种适合于野外简单条件下快速测定地质样品中铂和钯的分析方法。样品用盐酸-氯酸钾-氯化钠-氟化氢铵常温常压密闭分解，巯基棉分别富集铂和钯，灰化处理后采用三氯甲烷-石油醚（1：3）为萃取剂，DDO为显色剂萃取比色测定铂、钯的含量。巯基棉对钯的吸附率可达98%；加入氯化亚锡-水合肼（还原剂）使铂的吸附率提高到99%。方法检出限为Pt 0.05μg/g，Pd 0.02μg/g，标准物质的测定值与推荐值基本一致，野外地质样品的测定值与实验室分析结果吻合。
對于地毬化學樣品中鉑鈀的測定，傳統和現代分析方法均是建立在試金或樹脂及活性炭富集後用分光光度法或電感耦閤等離子體質譜法測定，而在野外滿足不瞭這些條件。本文基于樣品的性質及分光光度法的適應性彊等特點，開髮瞭一種適閤于野外簡單條件下快速測定地質樣品中鉑和鈀的分析方法。樣品用鹽痠-氯痠鉀-氯化鈉-氟化氫銨常溫常壓密閉分解，巰基棉分彆富集鉑和鈀，灰化處理後採用三氯甲烷-石油醚（1：3）為萃取劑，DDO為顯色劑萃取比色測定鉑、鈀的含量。巰基棉對鈀的吸附率可達98%；加入氯化亞錫-水閤肼（還原劑）使鉑的吸附率提高到99%。方法檢齣限為Pt 0.05μg/g，Pd 0.02μg/g，標準物質的測定值與推薦值基本一緻，野外地質樣品的測定值與實驗室分析結果吻閤。
대우지구화학양품중박파적측정，전통화현대분석방법균시건립재시금혹수지급활성탄부집후용분광광도법혹전감우합등리자체질보법측정，이재야외만족불료저사조건。본문기우양품적성질급분광광도법적괄응성강등특점，개발료일충괄합우야외간단조건하쾌속측정지질양품중박화파적분석방법。양품용염산-록산갑-록화납-불화경안상온상압밀폐분해，구기면분별부집박화파，회화처리후채용삼록갑완-석유미（1：3）위췌취제，DDO위현색제췌취비색측정박、파적함량。구기면대파적흡부솔가체98%；가입록화아석-수합정（환원제）사박적흡부솔제고도99%。방법검출한위Pt 0.05μg/g，Pd 0.02μg/g，표준물질적측정치여추천치기본일치，야외지질양품적측정치여실험실분석결과문합。
For the determination of Pt and Pd in geochemical samples,traditional and modern analytical methods are based on assaying or activated carbon and resin preconcentration and determination by Spectrophotometry and Inductively Coupled Plasma-Mass Spectrometry. However,these requirements cannot be met in the field. Based on the character of samples and the applicability of Spectrophotometry, this study develops a method in rapid determination of Pt and Pd in geochemical samples in the field. Samples are decomposed in the sealed Teflon container by the mixing of hydrochloric acid,potassium chlorate,sodium chloride,and ammonium hydrogen fluoride under normal temperature and pressure. Platinum and palladium are preconcentrated by sulfhydryl cotton. Pt and Pd are determined using chloroform petroleum and ether( 1 : 3 ) as the extractant,and DDO as the chromogenic agent. The adsorption capacity of sulfhydryl cotton for Pt can reach 98%,and the adsorption capacity of stannous chloride-drazine hydrate( reducing agent )for Pd can reach 99%. The detection limits of the method are 0. 05 μg/g and 0. 02 μg/g for Pt and Pd,respectively. The analytical values of standard materials, GBW07291,GBW07293,and GBW07341 are consistent with the respectively recommended values. The direct determination values of geological samples in the field are consistent with the results of laboratory analyses.
