DZT0064.75-1993地下水质检验方法射气法测定镭和氡.pdf 8页

'免费标准网(www.freebz.net)uz中华人民共和国地质矿产行业标准Dz/T0064.1一0064.80-93地下水质检验方法1993一02一27发布1993门0一01实施中华人民共和国地质矿产部发布免费标准网(www.freebz.net)无需注册即可下载 免费标准网(www.freebz.net)中华人民共和国地质矿产行业标准nz/T0064.75一93地下水质检验方法射气法测定镭和氨第一篇福，.1主题内容与适用范围本标准规定了射气法测定镭的方法。本标准适用于地下水中镭226的测定.1.2方法提要镭(zzsRa)属铀系元素，半衰期16ozy。在酸性溶液中，用钡盐作载体，使镭和硫酸钡形成同晶共沉淀。在碱性条件下，用乙二胺四乙酸二钠溶解，将溶液封存并经过一定时间使氧积累，通过测量氛222的放射性强度以测定镭。1.3仪器1.3.1氧牡分析器;自动定标器。1.3.2稳压电源。1.3.3真空泵。1.3.4玻璃扩散器(70-120mL),1.3.5仪器工作条件的选定:1.3.5.1测定本底与高压关系曲线。将高压由小往大调节，测出相应的本底值，绘制曲线供选择工作电压参考。1.3.5.2选定工作电压。用液体标准镭源测定不同高压下的脉冲频率，绘制“坪”压曲线。选取坪长的前号一合处的高压值作为工作电压比较合适。1.3.5.3选定甄别阀压。确定工作电压后，测出不同阀压的计数率，阀压一般选在2V左右，如阀压过低，灵敏度太高，干扰大仪器本底高。1.3.6仪器标定:使用的仪器及每个闪烁室，必须用2个不同数量级的液体标准镭源，采用真空法进行标定，以求得与测定样品相同条件下仪器的校正系数K值，并按式(1)计算:a一(1-e-")K=I式中:K—仪器校正系数,Ci/(脉冲·min-");a—液体标准镭源含量,Ci;I-镭源净计数率，脉冲/min;1-e-"止一氧积累函数(见表1)e中华人民共和国地质矿产部1993一02-27批准1993一10一01实施211免费标准网(www.freebz.net)无需注册即可下载 免费标准网(www.freebz.net)Dz/T0064.75一93表1氛1-e-li函数值时0I2345678910I1121314、00.0000.1660.3040.4200.5160.5960.6630.7190.7660.8040.8370.8640.8860.9050.92110.0080.1720.3090.4240.5190.5990.6660.7210.7670.8060.8380.8650.8870.9060.92220.0150.1780.3150.4280.5230.6020.6680.7230.7690.8070.8390.8660.8880.9070.922钾30.0220.1850.3200.4330.5270.6050.6710.7250.7710.8090.8410.8670.8890.9070.92340.0300.1910.3250.4370.5300.6080.6730.7270.7730.8100.8420.8680.8900.9080.92350.0370.1970.3300.4410.5340.6110.6760.7290.7740.8120.8430.8690.8910.9090.92460.0410.2030.3350.4450.5370.6140.6780.7310.7760.8130.8440.8700.8920.9090.92570.0520.2090.3400.4490.5410.6170.6800.7330.7780.8150.8450.8710.8920.9100.92580.0590.2150.3450.4540.5440.6200.6830.7350.7790.8160.8460.8720.8930.9110.92690.0660.2210.3500.4580.5470.6230.6850.7370.7810.8170.8480.8730.8940.9120.926100.0730.2270.3550.4620.5510.6250.6880.7390.7830.8190.8490.8740.8950.9120.927110.0800.2320.3600.4660.5540.6280.6900.7410.7840.8200.8500.8750.8960.9130.927120.0870.2380.3640.4700.5580.6310.6920.7430.7860.8210.8510.8760.8960.9140.928130.0940.2440.3690.4740.5610.6340.6950.7450.7870.8230.8520.8770.8970.9140.928140.1000.2500.3740.4780.5640.6370.6970.7470.7890.8240.8530.8780.8980.9150.929150.1070.2550.3790.4820.5680.6390.6990.7490.7910.8250.8540.8780.8990.915。.929一160.1140.2610.3830.4860.5710.6420.7010.7510.7920.8270.8550.8790.8990.9160.930170.1210.2660.3880.4890.5750.6450.7040.7530.7940.8280.8570.8800.9000.9170.931I80.1270.2720.3920.4930.5770.6470.7060.7550.7950.8290.8580.8810.9000.917190.1340.2770.3970.4970.5810.6500.7080.7570.7970.8310.8590.8820.9020.918200.1400.2830.4020.5010.5840.6530.7100.7580.7980.8320.8600.8830.9020.919210.1460.2880.4060.5050.5870.6550.7120.7600.8000.8330.8610.3840.9030.919220.1530.2940.4110.5080.5900.6580.7150.7620.8010.8340.8620.8850.9040.920230.1600.2990.4150.5120.5930.6610.7170.7640.8030.8350.8630.8860.9050.920一212免费标准网(www.freebz.net)无需注册即可下载 免费标准网(www.freebz.net)Dz/T0064.75一93积累(A=0.00755.h-")夜1516171吕1920212223242526272829300.9340.9450.9540.9620.9680.9730.9780.8910.9850.亏8?0.9890.9910.9930.9940.9950.9960.9350.9450.9540.9620.9680.9740.9780.9820.9850.9870.9890.9910.9930.9940.9950.9350.9460.9550.9620.9690.9740.9780.9820.9850.9870.9890.9910.9930.9940.9950.9360.9460.9550.9630.9690.974097台0.9820.9850.9870.9890.9910.9930.9940.99540.9360.9470.9560.963公.Q690.9740.9780.9820.9850.9870.990D.9910.9930.9940.9950.9360.9470.9560.9630.9690.9740.9790.9820.9850.9870.9900.9910.9930.9940.9950.9370.9470.9560.9630.9700.9750.9790.9820.9850.9880.9900.9910.9930.9940.9950.9370.9480.9570.9640.9700.9750.9790.9820.9850.9880.9900.9910.9930.9940.9950.9380.9480.9570.9640.9700.9750.9790.9830.9850.9880.9900.9920.9930.9940.9950.9380.9490.9570.9640.9700.9750.9790.9830.9860.9880.9900.9920.9930.9940.9950.9390.9490.9570.9650.9700.9750.9790.9830.9860.9880.9900.9920.9930.9940.9950.9390.9490.9580.9650.9710.9760.9800.9830.9860.9880.9900.9920.9930.9940.9950.9400.9500.9580.9650.9710.9760.9800.9830.9860:9880.9900-9920.9930.9940.9950.9400.9500.9580.9650.9710.9760.9800.9830.9860.9880.9900.9920.9930.9940.9950.9410,9510.9590.9660.9710.9760.9800.9830.9860.9880.9900.9920.9930.9940.9950.9410.9510.9590.9660.9720.9760.9800.9830.9860.998nq0nnOO，0.9930.9940.9950.9420.9510.9590.9660.9720.9760.9800.9840.9860.9890.9900.9920.9930.9940.9950.9420.9520.9600.9660.9720.9770.9800.9840.9860.9890.9910.9920.9930.9950.9950.9720.981八公会0n00"nOo，0.9420.9520.9600.9660.977仓9840.987‘J曰‘日JV.护J占、J习J司司0.9930.9950.9950.9430.9520.9600.9670.9720.9770.9810-9840.9870.9890.9910.992099今0.9950.9950.9430.9530.9610.9670.9730.9770.9810.9840.9870.9890.9910-9920.9940.9950.9960.9440.9530.9610.9670.9730.9770.9810.9840.9870.9890.9910.9920.9940.9950.9960.9440.953096王0.9680.9730.9770.9810.9840.9870989n_9910.9920.9940.9950.9960.9450.9540.9610.9680.9730.9780.9810.9840.9870.9890.9910.9920.99409950.996213免费标准网(www.freebz.net)无需注册即可下载 免费标准网(www.freebz.net)DZ/T0064.75一931.4试剂1.4.1甲基橙溶液(10g/L),1.4.2氯化钡溶液(50g/L),1.4.3硫酸溶液(1+D.1.4.4盐酸溶液(1+1),1.4.5胳香草酚蓝乙醇溶液(1g/L)a1.4.6氢氧化钠溶液(2oog/L及50g/L).1.4.7乙二胺四乙酸二钠。1.4.8液体标准镭源,nX10-"0ci及.Xlo-1"ci15分析步骤1.5.1样品处理:取水样500mL，加甲基橙溶液(1.4.1)2滴，用盐酸溶液(1.4.2)中和至红色，煮沸几分钟，加硫酸溶液(1.4.3)2mL，在搅拌下滴加氯化钡溶液(1.4.4)2mL，保温几小时或放置过夜。用双层中速定量滤纸过滤，用纯水将沉淀洗几次后冲人原烧杯(体积约100mL左右)，加乙二胺四乙酸二钠2g,察香草酚蓝溶液(1.4.5)5滴，用氢氧化钠溶液(1.4.6)中和至深蓝色，煮沸至沉淀完全溶解，溶液应清澈透明。再蒸发浓缩体积至约30^-50mL，冷却。将浓缩液全部转入扩散器中，用少量纯水洗涤烧杯3次，溶液并入扩散器。用真空泵排除氧气，在负压下封存样品，记录日期，积累20-30d，按射气法测定镭含量。1.5.2测量:选取与标定仪器相同条件测定本底计数率(脉冲/min)，取10次读数的平均值。按真空泵功率大小，确定抽气时间的长短，达到一定的真空度后，关闭进气孔，连接扩散器，依次打开管夹，慢慢旋开扩散器顶部的螺旋夹，将氛气引入闪烁室。水样经过真空扩散脱气，使氧气与水分离，掌握好鼓泡速度，脱气15min左右。在氛气输入30min开始正式计数，一般选取10次读数平均值。16分析结果的计算按式(2)计算镭含量:Ra一;鬓李共毕X3.7X10"0⋯，......·.........⋯⋯‘...⋯⋯(2)‘“V·(1-e-")‘“一’‘’一’一‘式中:Ra—水样中镭含量，鞠/L;K—仪器校正系数.Ci/(脉冲加in");I—样品加本底的计数率，脉冲/min;I,—本底计数率，脉冲/min;v—取水样体积，L;1-e--氛积累函数(查附表1).第二篇氮21主题内容与适用范围本标准规定了用射气闪烁法测定地下水中氛的方法。本标准适用于地下水中氧的测定.22方法提要氛(""Rn)是天然，xen系中，"Ra的衰变产物，半衰期3.825a，比重0.0096g/cm"。在水中有一定的溶解度，其溶解系数与水的温度关系密切，随温度升高而减小。通过氧及其子体衰变时放出的。粒子在ZnS(Ag)闪烁室中引起的闪光，经光电转换放大，形成电脉冲，单位时间内产生的脉冲数与氛浓度成正比。2.3仪器2.3.1X闪烁计数器及配套自动定标器214免费标准网(www.freebz.net)无需注册即可下载 免费标准网(www.freebz.net)DZ/T0064.75一932.3.2真空泵2.3.3玻璃扩散器2-4分析步骤2.4.1测本底值，选取与标定仪器相同条件测定本底计数率(脉冲/min)，取10次读数的平均值。2.4.2抽真空，按真空泵功率大小，确定抽气时间的长短，达到一定的真空度后，关闭进气孔，连接盛装样品的扩散器，依次打开管夹，慢慢旋开扩散器顶部的螺旋夹，借助压差，将氛气引入闪烁室。2.4.3脱气，水样经过真空扩散脱气，使氛气与水分离，掌握好鼓泡速度，脱气15min左右。2.4.4读数，根据氮及其子体的衰变规律在氧气输入30min开始正式计数，一般选取10次读数平均值。2-5氛的含量按下式计算:QR。一典奥乒X3.7X10"0犷一七式中:Q、—水样中氧含量,助/L;K-仪器校正系数，(Ci/(脉冲。min-");N—样品加本底的计数率，脉冲/min;。—本底计数率，脉冲/min;v—取水样体积，L;e-a}-氧衰变函数(见表2).免费标准网(www.freebz.net)无需注册即可下载 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免费标准网(www.freebz.net)DZ/T0064.75-93附加说明:本标准由地质矿产部提出。本标准由地质矿产部水文地质工程地质研究所归口。本标准由地质矿产部水文地质工程地质研究所负责起草。本标准主要起草人李正清。免费标准网(www.freebz.net)无需注册即可下载'