生态环境学报
生態環境學報
생태배경학보
ECOLOGY AND ENVIRONMENT
2013年
11期
1841-1845
,共5页
张雪霞%张晓霞%陈能场%郑煜基%李金娟
張雪霞%張曉霞%陳能場%鄭煜基%李金娟
장설하%장효하%진능장%정욱기%리금연
硫%铁%比浊法
硫%鐵%比濁法
류%철%비탁법
sulfur%iron%spectroscopic barium turbidimetry
硫酸钡分光光度比浊法是大批量测定土壤环境样品硫含量的常用方法,但影响测定结果的因素较多,如稳定剂的选择、酸度的控制、BaC12的形态和用量等均可对测定结果产生影响。在多金属硫化物矿区,由于长期的采矿冶炼活动,造成周边土壤中硫、铁含量增加,用比浊法测定硫含量时,铁的含量也对测定结果产生显著影响。针对这些影响因素,本研究在用硝酸-高氯酸湿法对土壤进行消解后,优化了硫酸钡分光光度比浊法测定高硫高铁样品的实验条件和实验步骤,并对多金属硫化物矿区的土壤样品进行了测定,得到了较好的结果。实验证明,称取0.50 g土壤样品,消解后过滤,取滤液7 mL,加入1 mL ?[(1+2)甘油-乙醇]=6%的甘油-乙醇为稳定剂,1 mL 浓磷酸掩蔽 Fe3+与 Cl-反应所显的黄色,定容到10 mL,加入w(BaCl2)=10%的氯化钡溶液10 mL,电磁搅拌1 min,静置20~40 min,在波长440 nm处,比浊法测定土壤全硫含量,相对误差<10%,取得良好的测定结果。此方法简单、快捷、方便,适合大批量环境样品的测定。
硫痠鋇分光光度比濁法是大批量測定土壤環境樣品硫含量的常用方法,但影響測定結果的因素較多,如穩定劑的選擇、痠度的控製、BaC12的形態和用量等均可對測定結果產生影響。在多金屬硫化物礦區,由于長期的採礦冶煉活動,造成週邊土壤中硫、鐵含量增加,用比濁法測定硫含量時,鐵的含量也對測定結果產生顯著影響。針對這些影響因素,本研究在用硝痠-高氯痠濕法對土壤進行消解後,優化瞭硫痠鋇分光光度比濁法測定高硫高鐵樣品的實驗條件和實驗步驟,併對多金屬硫化物礦區的土壤樣品進行瞭測定,得到瞭較好的結果。實驗證明,稱取0.50 g土壤樣品,消解後過濾,取濾液7 mL,加入1 mL ?[(1+2)甘油-乙醇]=6%的甘油-乙醇為穩定劑,1 mL 濃燐痠掩蔽 Fe3+與 Cl-反應所顯的黃色,定容到10 mL,加入w(BaCl2)=10%的氯化鋇溶液10 mL,電磁攪拌1 min,靜置20~40 min,在波長440 nm處,比濁法測定土壤全硫含量,相對誤差<10%,取得良好的測定結果。此方法簡單、快捷、方便,適閤大批量環境樣品的測定。
류산패분광광도비탁법시대비량측정토양배경양품류함량적상용방법,단영향측정결과적인소교다,여은정제적선택、산도적공제、BaC12적형태화용량등균가대측정결과산생영향。재다금속류화물광구,유우장기적채광야련활동,조성주변토양중류、철함량증가,용비탁법측정류함량시,철적함량야대측정결과산생현저영향。침대저사영향인소,본연구재용초산-고록산습법대토양진행소해후,우화료류산패분광광도비탁법측정고류고철양품적실험조건화실험보취,병대다금속류화물광구적토양양품진행료측정,득도료교호적결과。실험증명,칭취0.50 g토양양품,소해후과려,취려액7 mL,가입1 mL ?[(1+2)감유-을순]=6%적감유-을순위은정제,1 mL 농린산엄폐 Fe3+여 Cl-반응소현적황색,정용도10 mL,가입w(BaCl2)=10%적록화패용액10 mL,전자교반1 min,정치20~40 min,재파장440 nm처,비탁법측정토양전류함량,상대오차<10%,취득량호적측정결과。차방법간단、쾌첩、방편,괄합대비량배경양품적측정。
Spectroscopic barium turbidimetry (SBT) is commonly used in determining the content of sulfur in the soil samples, which was influenced by the stabilizers, acidity, and the forms of adding BaCl2, etc. The long-term mining and metallurgical activities have resulted in the generation of huge amounts of mine wastes including acid-generating sulfuric tailings and acid mine drainage (AMD). They lead to the increase of the concentration of sulfur and iron in the surrounding environment. And the higher concentration of Fe3+ will disturb the determination of sulfur for the formation of color. The aim of this study was to improve conditions and procedures of operation for sulfur determination with SBT method, so that this method could be used in the high-sulfur and high-iron soil samples. At first, 0.50 g of soil samples were digested using HNO3-HClO4 and made up to 25 mL. 7 mL of the digestion solution was added 1 mL of (1+2) glycerol-ethanol solution (?=6%) as stabilizer and 1 mL concentrated phosphoric acid as masking agent which masked yellow colour caused by Fe3+and Cl-reaction. The mixture was made up to 10 mL and then transferred into a 50 mL beaker. After adding 10 mL of BaCl2 solution (w=10%) and electromagnetic stirring for 1 min, total sulfur in the soil was determined between 20 minutes and 40 minutes at 440 nm wavelength. The result showed that the relative error was less than 10%, which suggested that the modified turbidimetry could be applied to determine the sulfur content in high-sulfur and high-iron soil samples.