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煤中砷測定儀器
2021-08-17 來自: lmsjdb.cn 瀏(liu)覽次數:412
煤中砷測定儀器工作曲線的繪制：
分別用(yong)(yong)單刻(ke)度移液(ye)(ye)(ye)(ye)管吸(xi)(xi)取0．00ml,1.00ml,2.00ml.3.00ml.4.00ml.5.00ml,的砷標準溶(rong)(rong)液(ye)(ye)(ye)(ye)于砷測(ce)(ce)定(ding)儀圓燒瓶(ping)中(zhong)(zhong)，先加(jia)人10ml(6mol/L)硫(liu)酸(suan)(suan)(suan)溶(rong)(rong)液(ye)(ye)(ye)(ye)，再加(jia)入(ru)(ru)(ru)20 mL(6mol/L)鹽酸(suan)(suan)(suan)溶(rong)(rong)液(ye)(ye)(ye)(ye)，用(yong)(yong)水稀釋至(zhi)(zhi)50ml。然后加(jia)入(ru)(ru)(ru)2ml碘化(hua)鉀溶(rong)(rong)液(ye)(ye)(ye)(ye)，1ml氯化(hua)亞錫溶(rong)(rong)液(ye)(ye)(ye)(ye)，搖勻，在室溫(wen)下放置15min。用(yong)(yong)移液(ye)(ye)(ye)(ye)管往(wang)砷測(ce)(ce)定(ding)儀吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)器中(zhong)(zhong)加(jia)入(ru)(ru)(ru)3ml碘溶(rong)(rong)液(ye)(ye)(ye)(ye)，1ml碳酸(suan)(suan)(suan)氫(qing)鈉(na)溶(rong)(rong)液(ye)(ye)(ye)(ye),6ml水，將吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)器插入(ru)(ru)(ru)裝有乙酸(suan)(suan)(suan)鉛棉的吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)器套管中(zhong)(zhong)。往(wang)圓燒瓶(ping)中(zhong)(zhong)加(jia)入(ru)(ru)(ru)5.0g無砷金屬鋅，立即將吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)器套管與燒瓶(ping)連接好，確認儀器各接口不漏氣(qi)后，讓發生過(guo)程持續約1h.取出吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)器，加(jia)入(ru)(ru)(ru)5 ml鉬酸(suan)(suan)(suan)銨一硫(liu)酸(suan)(suan)(suan)肼混合(he)溶(rong)(rong)液(ye)(ye)(ye)(ye)，并用(yong)(yong)洗耳(er)球從吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)器側(ce)孔往(wang)內打氣(qi)約10次，使吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)液(ye)(ye)(ye)(ye)充分混合(he)均勻。將吸(xi)(xi)收(shou)(shou)(shou)(shou)(shou)(shou)器放在沸騰的水浴中(zhong)(zhong)加(jia)熱20min，取出，冷卻至(zhi)(zhi)室溫(wen)。
在分光光度計上，用10mm比色皿于830 nm(或(huo)700 nm)波(bo)(bo)長(chang)(chang)下以(yi)標準空白溶(rong)液為參比，測(ce)量各標準溶(rong)液的吸(xi)(xi)光度。相同濃度的砷在830 nm波(bo)(bo)長(chang)(chang)下吸(xi)(xi)光度是(shi)700nm波(bo)(bo)長(chang)(chang)下吸(xi)(xi)光度的3倍左(zuo)右，煤中砷含量較(jiao)低時，在830 nm波(bo)(bo)長(chang)(chang)下測(ce)定(ding)吸(xi)(xi)光度。
以標(biao)(biao)準系列溶液中砷質量(pg)為橫(heng)坐標(biao)(biao)，相應(ying)的(de)吸(xi)光(guang)度(du)為縱(zong)坐標(biao)(biao)，繪(hui)制(zhi)(zhi)工作(zuo)曲線(xian)。繪(hui)制(zhi)(zhi)工作(zuo)曲線(xian)應(ying)與煤樣分析同時進行，每次測定應(ying)繪(hui)制(zhi)(zhi)工作(zuo)曲線(xian)。
工作曲線一年一次。