1、铁的测定数据记录铁的测定数据记录制备标准储备液:称取NH4Fe(SO4)212H2O 0.8658g用水溶解再加0.25ml HNO3,用5%的HNO3稀释制备成1mg/ml的铁溶液。1、铁浓度测定序号测量对象样品编号Abs浓度实际浓度SDRSD%日期时间1标准样品Fe10.115910.00151.25942011/7/511:242标准样品Fe20.315330.00230.73732011/7/511:253标准样品Fe30.443250.00360.80532011/7/511:264标准样品Fe40.548470.00240.43142011/7/511:285标准样品Fe50.63
2、890.00250.39372011/7/511:306样品水样1取10ml储备液稀释成100g/ml的标准使用液,再分别取1ml ,3ml ,5ml ,7ml, 9ml的标准使用液将其分别稀释成1ug/ml、3 ug/ml、5 ug/ml、7 ug/ml、9 ug/ml的标准溶液系列,用火焰原子吸收光谱。仪测得结果如下表:2、增敏剂加入测量分别制备4组7 ug/ml的铁溶液,1组7 ug/ml空白对照,2、3、4组分别加入10ml 0.01g/ml 序号测量对象样品编号Abs浓度实际浓度SDRSD%日期时间1标准样品Fe0.427170.00350.82162011/7/512:432标准样
3、品Fe+SDS0.553470.00360.64322011/7/512:453标准样品Fe+8-羟基喹啉0.421570.00350.82542011/7/512:464标准样品Fe+6次甲基4胺0.485970.00370.7532011/7/512:475样品水样13、低浓度铁标准溶液测定再用储备液配置铁溶液为10ug/ml的稀溶液用10ug/ml的稀溶液将铁分别稀释成0.1ug/ml、0.3 ug/ml、0.5 ug/ml、0.7 ug/ml、0.9 ug/ml用火焰原子吸收光谱,仪测得结果如下表:序号测量对象样品编号Abs浓度实际浓度SDRSD%日期时间1标准样品Fe10.00960
4、.10.00066.03962011/7/512:542标准样品Fe20.03330.30.00072.02252011/7/512:553标准样品Fe30.05480.50.00162.8392011/7/512:564标准样品Fe40.07380.70.00060.8682011/7/512:585标准样品Fe50.09410.90.0011.01792011/7/512:596样品水样14、低浓度铁标准溶液加入10ml 0.01g/ml增敏剂的测定分别制备3组0.7 ug/ml的铁溶液,1组0.7 ug/ml空白对照,2、3组分别加入10ml 0.01g/ml SDS和六次甲基四胺。测定
5、结果如下表:序号测量对象样品编号Abs浓度实际浓度SDRSD%日期时间1标准样品Fe0.09460.70.00131.41672011/7/513:312标准样品Fe+SDS0.12840.70.0032.35442011/7/513:323标准样品Fe+6次甲基4胺0.10830.70.00131.24462011/7/513:344样品水样15、低浓度铁标准溶液加入5ml 0.01g/ml增敏剂的测定分别制备3组0.7 ug/ml的铁溶液,1组0.7 ug/ml空白对照,2、3组分别加入5ml 0.01g/ml SDS和六次甲基四胺。测定结果如下表:序号测量对象样品编号Abs浓度实际浓度S
6、DRSD%日期时间1标准样品Fe0.09610.70.00242.50792011/7/513:392标准样品Fe+SDS.50.11070.70.00222.00412011/7/513:413标准样品Fe+6次.50.09980.70.0021.9552011/7/513:424样品水样1实验表明SDS对铁的增敏效果良好,所以选择SDS做为增敏剂。1ug/ml、3 ug/ml、5 ug/ml、7 ug/ml、9 ug/ml的标准溶液系列测得的线性关系:0.1ug/ml、0.3 ug/ml、0.5 ug/ml、0.7 ug/ml、0.9 ug/ml的铁标准溶液系列测得的线性关系: 时间:20
7、11年7月5日铁的测定数据记录2011年7月6日称取硫酸铁铵的质量为0.8686g,溶解于5%的硝酸,并用5%的硝酸稀释定容至100ml,浓度约为1mg/ml,其为铁的标准贮液1)取1ml铁的标准贮液稀释为10 g/ml 的标准使用液,分别取1ml,3ml,5ml, 7ml,9ml的10 g/ml 的标准使用液稀释为以下浓度:0.1,0.3,0.5,0.7,0.9ug/ml浓度(ug/ml)吸光度ASDRSD%0.10.02260.00031.48160.30.05040.00081.55550.50.07340.00081.0770.70.10090.00070.72650.90.12670
8、.00070.5603线性关系如下:2)取10ml铁的标准贮液稀释为10 0g/ml 的标准使用液,分别取1ml,3ml,5ml, 7ml,9ml的100 g/ml 的标准使用液稀释为以下浓度:1,3,5,7,9ug/ml:浓度(ug/ml)吸光度ASDRSD%10.07230.0011.314330.18380.00120.635750.27680.00070.250370.3620.00160.443490.45730.00430.9296线性关系如下:取稳定的浓度5g/ml的铁标液加入不同量的增敏剂SDS如下:体积/mlAbsSDRSD%00.30350.00331.078810.300
9、30.00250.828130.31890.00260.806850.33920.00260.759870.35770.00320.899890.34050.00160.4806110.35570.00290.8096130.34790.00170.4999150.34560.00130.3861170.34420.00160.4774变化趋势如下:或0.9g/ml的铁标液加入不同量的增敏剂SDS:SDS体积/mlAbsSDRSD%00.12820.00896.941910.12910.00493.761130.13930.00392.775950.14280.00372.586370.153
10、30.0031.952390.17930.00522.8911110.15860.00271.7123130.11030.00121.0842150.06240.00091.4594170.05020.00050.9555图如下:或实验表明:铁的线性范围在0-1g/ml线性比较好,且在0.9g/ml的铁标液时最稳定,故取0.9g/ml的铁标液与SDS不同量的加入测定其吸光度,得出SDS加入量为9-10ml时增敏效果最好,增敏效果为39.86%.增敏效果=(加入增敏剂后的吸光度-加入前的吸光度)/加入前的吸光度铁的测定数据记录(2011.7.8)称取0.8694g硫酸铁铵,加入少许蒸馏水溶解,再
11、用5%的稀硝酸稀释定容在100ml中做贮液,浓度为1.0mg/ml.取5ml的贮液稀释到500mL的瓶中配成10g/ml的标准使用液,取1ml,3ml,5ml, 7ml,9ml的10 g/ml 的标准使用液稀释为以下浓度:0.1,0.3,0.5,0.7,0.9ug/ml标准曲线为如下:Abs浓度SDRSD%0.02980.10.0013.27510.04750.30.00071.51880.06840.50.00152.16010.08670.70.00070.75510.10710.90.00211.9967曲线如下:不同增敏剂的量与吸光度的关系:溴化铵的浓度为10g/ml样品编号Abs浓度
12、SDRSD%Fe空白0.082500.00060.7072Fe+溴化铵3ml0.08830.00030.3083Fe+溴化铵5ml0.0950.00030.2954Fe+溴化铵7ml0.091670.00060.6888Fe+溴化铵9ml0.095690.00080.8652Fe+溴化铵11ml0.0903110.00040.4721Fe+溴化铵13ml0.0891130.00060.7249Fe+溴化铵15ml0.0812150.00182.2594SDS的不同量加入的影响样品编号Abs体积(ml)SDRSD%Fe空白0.062500.0011.5859Fe+SDS3ml0.069830.0
13、011.3668Fe+SDS5ml0.074450.00091.1483Fe+SDS7ml0.079970.00050.6757Fe+SDS9ml0.095590.00262.7096Fe+SDS11ml0.0782110.00070.8372Fe+SDS13ml0.0774130.00111.4347Fe+SDS15ml0.0717150.00070.9446十六烷基三甲基溴化铵的不同加入量:样品编号Abs浓度SDRSD%Fe空白0.076600.00060.7532Fe+16烷基3甲基溴化铵3ml0.079630.00030.3738Fe+16烷基3甲基溴化铵5ml0.082850.000
14、50.5744Fe+16烷基3甲基溴化铵7ml0.085370.00050.5438Fe+16烷基3甲基溴化铵9ml0.084890.00030.404Fe+16烷基3甲基溴化铵11ml0.0818110.00070.8852Fe+16烷基3甲基溴化铵13ml0.0765130.00060.8185Fe+16烷基3甲基溴化铵15ml0.0725150.00010.2024曲线图如下:8-羟基喹啉不同加入量:样品编号Abs浓度SDRSD%Fe空白0.063800.00050.8378Fe+8羟基喹啉3ml0.074530.00050.6988Fe+8羟基喹啉5ml0.065350.00111.6
15、748Fe+8羟基喹啉7ml0.065770.00030.4882Fe+8羟基喹啉9ml0.067390.00030.506Fe+8羟基喹啉11ml0.068110.00081.1982Fe+8羟基喹啉13ml0.0684130.00040.5605Fe+8羟基喹啉15ml0.0721150.00030.4342Fe+8羟基喹啉17ml0.0614170.00142.233Fe+8羟基喹啉19ml0.0612190.00030.5112曲线图如下:六次甲基四铵加入的不同量:样品编号Abs浓度(10ug/ml)SDRSD%Fe空白0.074200.00162.1951Fe+6次甲基3ml0.07
16、6230.00030.4518Fe+6次甲基5ml0.077950.00040.4999Fe+6次甲基7ml0.079270.00020.2847Fe+6次甲基9ml0.086690.00121.406Fe+6次甲基11ml0.0743110.00060.7617Fe+6次甲基13ml0.0738130.00091.1691Fe+6次甲基17ml0.0725150.00070.9853曲线如下铁的测定数据记录(2011.7.9)酸度的选择:加入不同的硫酸量(1+10),将稳定浓度时铁标液的铁的量与不同酸的量混合用蒸馏水稀释到100ml的容量瓶中如下:Abs硫酸的体积/ml SDRSD%0.09
17、4510.0011.10370.094130.00020.21010.095150.00151.59540.096170.0011.03030.097890.00080.84670.0985110.00080.82890.0994130.00050.5110.0996150.00030.32180.0996170.00141.38220.0989190.00050.4611加入不同的硝酸量(1+10),将稳定浓度时铁标液的铁的量与不同酸混合用蒸馏水稀释到100ml的容量瓶中如下:体积/mlAbsSDRSD%10.10340.00121.131230.09750.00040.41350.0973
18、0.00040.362970.0970.00030.306590.10260.00030.2477110.09710.00020.1939130.102330.00040.3698150.09480.00030.2733170.09470.00030.2956190.09450.00060.6143250.09480.00040.4421300.09260.00090.9291350.09420.00050.5141400.09550.00020.2206450.09510.00030.3003加入不同的盐酸量(1+10),将稳定浓度时铁标液的铁的量与不同酸混合用蒸馏水稀释到100ml的容量瓶
19、中如下:体积/ml AbsSDRSD%10.0790.00111.425630.08770.00141.564150.09060.00060.663970.09380.00040.435390.09690.00080.8057110.09670.00070.723130.09660.00111.1903150.09730.00030.319170.09850.00070.6673190.09770.00040.3715铜的标液测定称取0.1060g的铜粉用少量的水稀释后,用(1+1)的硝酸溶解,再用5%的稀硝酸稀释到浓度为1mg/ml的贮备液,取5ml的贮备液到500ml的容量瓶中用5%的稀硝酸定容,其浓度为10g/ml 的标准使用液,分别取1ml,3ml,5ml, 7ml,9ml的10 g/ml 的标准使用液稀释为以下浓度:0.1,0.3,0.5,0.7,0.9ug/ml作标准曲线:浓度AbsSDRSD%0.10.03440.00061.88150.30.07720.00030.41670.50.12240.00060.4730.70.16890.00070.40850.90.21420.0052.3546 铁标准曲线酸度增敏剂
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