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土壤中有毒元素的测定结果
浏览次数:511发布日期:2018-12-26

【LAIYUAN/ZUOZHE】BEINACHUANGLIAN 

水系沉积物

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2JIEGUOYUTAOLUN

懂球帝2.1YANGPINCHULITIAOJIANYOUHUA

按照笔者前期对水系沉积物懂球帝处理的方法对土壤样品前处理条件进行优化试验,以称样量、溶剂用量、溶剂种类、消解时间和消解温度5个条件为考察对象。其中消解时间:3,6,8,10,12,16,20,24h;消解温度:100,120,140,160,180℃;溶剂:盐酸、硝酸、盐酸+过氧化氢、王水和逆王水;溶剂用量:1,2,3mL。

2.1.1CHENGYANGLIANG

试验发现,称样量较大时,溶剂对样品的溶解效果很差。主要是因为消解内罐容积较小(10mL),能加入的消解溶剂较少,高温高压条件下如果消解溶剂量超过内罐溶剂四分之一便会产生泄露和爆炸的危险。当称样量为0.010g时溶解效果较好。

2.1.2RONGJIYONGLIANG

RONGJIYONGLIANGSHIXIAOJIEYANGPINDEGUANJIAN,FENBIEQU1,2,3mLWANGSHUI,ZAI170℃DUITURANGBIAOZHUNFENTIJIAREXIAOJIE6h。JIEGUOFAXIAN,ZHUANGYOU1mLWANGSHUIDEGUANZHONGFENTICANZHAJIAODUO,DANZHUANGYOU3mLWANGSHUIDEGUANYOUXIELU,ZHUYAOSHIYINWEIRONGJILIANGYUEDA,GAOWENXIAGUANNEIYALIYUEDA,YIDANCHAOGUOGUANTIDEDACHENGSHOUYALIYETIJIUHUIXIELU,SHENZHISHIGUANTIFASHENGBIANXING。YINCIWEIQUEBAOGAOWENGAOYATIAOJIANXIAYANGPINWANQUANXIAOJIE,TONGSHIYOUBIMIANRONGJILIANGGUODUOERCHANSHENGXIELUHUOBAOZHADEWEIXIAN,HOUXUANZEZHURONGJIYONGLIANGWEI2mL。

2.1.3XIAOJIERONGJIZHONGLEI

固定称样量0.010g,溶剂用量2mL,170℃加热消解6h,分别考察盐酸、硝酸、盐酸–0.5mL过氧化氢、王水和逆王水对土壤标准粉体中重金属的提取情况。结果表明,使用单一酸HCl或HNO3对土壤样品的消解能力没有使用混酸时效果好。但是加入过氧化氢时内罐有些许泄露,因为H2O2作为消解试剂时,即使在较低的温度下也能分解出高能态活化氧,产生大量气泡,而高压密闭内罐体积仅10mL,所以容易带着粉末样品冲出容器而造成泄漏。逆王水的消解效果比传统王水的消解效果好。因此选择HCl与HNO3的体积比为1∶3的逆王水(0.5mLHCl+1.5 mL HNO3)作为土壤的消解溶剂。

2.1.4XIAOJIEWENDU

GUDINGCHENGYANGLIANG0.010g、RONGJINIWANGSHUI2mL、XIAOJIE6hBUBIANDETIAOJIANXIA,FENBIEKAOCHABUTONGWENDUXIAYANGPINDEXIAOJIEQINGKUANG。JIEGUOBIAOMING,DANGXIAOJIEWENDUCHAOGUO160℃SHI,YANGPINRONGJIEWANQUANQIEBUXIELU。WEIJIEYUENENGYUANXUANZE160℃WEIXIAOJIEWENDU。

2.1.5XIAOJIESHIJIANXUANZE

懂球帝GUDINGQITATIAOJIANBUBIANFENBIEKAOCHABUTONGSHIJIANXIAYANGPINDEXIAOJIEQINGKUANG。JIEGUOBIAOMING,DANGXIAOJIESHIJIANCHAOGUO6hSHI,YANGPINRONGJIEWANQUAN,RONGYECHENGQIANHUANGLVSE,JINGICP–MSJIANCE,GEZHONGJINSHUHANLIANGYUGUOBIAOTUIJIANZHIXIANGFU。WEICHONGFENXIAOJIEYANGPINYOUJIESHENGSHIJIANYIBIANYUPILIANGCHULI,XUANZEXIAOJIESHIJIANWEI6h。ZONGHEKAOLV,SHIYANXUANZECHENGYANGLIANGWEI0.0100g,YONG2mLNIWANGSHUIZUOWEIXIAOJIERONGJIZAI160℃XIAXIAOJIE6h。

懂球帝2.2YIQIDEDIAOXIEHEZHILIANGSHUDEXUANZE

懂球帝YIQIDIANHUOHOU,WENDINGYUE30min,DENGWUHUAQIWENDUJIANGZHI2℃ZUOYOU,YONGDIAOXIEYEDIAOXIE,DAIDIAOXIEYUANSULINGMINDU、WENDINGXING、YANGHUAWUHESHUANGDIANHEDENGZHIBIAODADAOSHI,QUEDING1.2ZHONGDEYIQIGONGZUOCANSHU。LINGWAI,DAICEYUANSUZHILIANGSHUDEXUANZESHIXIAOCHUGANRAO、TIGAOCEDINGLINGMINDUDEZHUYAOYINSUZHIYI,YINWEIDADUOSHUYUANSUDOUJUYOUTONGWEISU,ZAIICP–MSCEDINGZHONGXUANZEYUANSUZHILIANGSHUDEMUDESHIWEILEBIKAITONGZHIYIWEISUHEYANGHUAWUDENGDUOYUANZILIZIDEGANRAO,TONGSHIHAIYAOBAOZHENGYUANSUDEFENGDUHELINGMINDUGAO。GENJUSHIYANJIANCEJIEGUO,XUANZEFENGDUGAOQIELINGMINDUXIANGDUIJIAOGAODEDAICEYUANSUTONGWEISU,FENBIEWEI52Cr,63Cu,7s,111Cd,202Hg,208Pb。

2.3XIANXINGFANGCHENGYUJIANCHUXIAN

准确配制各元素质量浓度均为0,0.5,5,10,20μg/L的系列标准溶液,在1.2仪器工作条件下,测定不同浓度下各元素对应的信号强度,以元素懂球帝的质量浓度X为横坐标、信号强度Y为纵坐标绘制标准工作曲线,得6种元素的线性方程,线性范围均为0~20μg/L。根据规定,在1.2仪器工作条件下,连续测定空白溶液11次,计算测定结果的标准偏差S,按3.143S计算方法检出限。线性方程、线性相关系数与检出限见表1。

2.4JINGMIDUYUZHUNQUEDUSHIYAN

ANSHIYANFANGFACEDINGLIANGZHONGTURANGCHENGFENGUOJIAYIJIBIAOZHUNWUZHI,CEDINGJIEGUOJIANBIAO2。YOUBIAO2KEZHI,GEYUANSUCEDINGJIEGUOYUBIAOZHUNZHIWENHE,CEDINGJIEGUODEXIANGDUIBIAOZHUNPIANCHAWEI1.3%~5.6%,SHUOMINGGAIFANGFADEZHUNQUEDUHEJINGMIDUJIAOHAO。

2.5JIABIAOHUISHOUSHIYAN

懂球帝DUITURANGYANGPINJINXINGJIABIAOHUISHOUSHIYAN,JINYIBUKAOCHAFANGFADEZHUNQUEDU,JIEGUOJIANBIAO3。CONGBIAO3ZHONGKEYIKANCHU,TURANGYANGPINDEJIABIAOHUISHOULVWEI91.2%~104.6%MANZUHUISHOULVYAOQIU,JINYIBUYANZHENGLEGAIFANGFADEZHUNQUEDUJIAOGAO。

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