海洋学研究 ›› 2023, Vol. 41 ›› Issue (3): 92-100.DOI: 10.3969/j.issn.1001-909X.2023.03.009
海水基质活性磷酸盐标准物质研制
张川1,2(
), 于涛1,2, 于小焱1,2, 朱勇3,4, 王丽芳5, 张晓慧1,2
- 1.国家海洋标准计量中心,天津 300112
2.海洋计量检测技术创新中心,天津 300112
3.自然资源部第二海洋研究所, 浙江 杭州 310012
4.自然资源部海洋生态系统动力学重点实验室,浙江 杭州 310012
5.厦门大学 近海海洋环境科学国家重点实验室,福建 厦门 361102
-
收稿日期:2023-01-19修回日期:2023-03-18出版日期:2023-09-15发布日期:2023-10-24 -
作者简介:张川(1981—),男,天津市人,高级工程师,主要从事海洋仪器设备校准技术及海洋标准物质研制方面的研究, E-mail:zhangchuan@ncosm.org.cn。 -
基金资助:自然资源部计量检测及质量监督资助项目(121154000000190010)
Preparation of standard reference material for reactive phosphorus with seawater matrix
ZHANG Chuan1,2(), YU Tao1,2, YU Xiaoyan1,2, ZHU Yong3,4, WANG Lifang5, ZHANG Xiaohui1,2
- 1. National Center of Ocean Standards and Metrology, Tianjin 300112, China
2. Technology Innovation Center for Marine Metrology and Instruments Test, MNR, Tianjin 300112, China
3. Second Institute of Oceanography, MNR, Hangzhou 310012, China
4. Key Laboratory of Marine Ecosystem Dynamics, MNR, Hangzhou 310012, China
5. State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361102, China
-
Received:2023-01-19Revised:2023-03-18Online:2023-09-15Published:2023-10-24
摘要：
本研究以西太平洋表层海水为基质,制备了浓度为0.5~4.0 μmol/L的海水活性磷酸盐系列标准物质。通过对所研制的4批次样品进行均匀性、稳定性评估,确定样品性能良好。对基于磷钼蓝分光光度法的气泡间隔连续流动分析系统的反应和操作条件进行优化,优化后的方法检出限低至0.03 μmol/L。不同浓度样品的相对标准偏差为0.37%~2.45%(n=9);通过与国际已有有证标准物质比对,本研究方法测量误差小于0.05 μmol/L。经6家具有中国计量认证资质且具备海水磷酸盐检测能力的实验室联合定值,确定了该系列标准物质的标准值,并对定值结果的不确定度进行了分析评价,相对扩展不确定度为2%~10%。
中图分类号:
引用本文
张川, 于涛, 于小焱, 朱勇, 王丽芳, 张晓慧. 海水基质活性磷酸盐标准物质研制[J]. 海洋学研究, 2023, 41(3): 92-100.
ZHANG Chuan, YU Tao, YU Xiaoyan, ZHU Yong, WANG Lifang, ZHANG Xiaohui. Preparation of standard reference material for reactive phosphorus with seawater matrix[J]. Journal of Marine Sciences, 2023, 41(3): 92-100.
图1 抗坏血酸质量浓度条件优化结果 (图中数据点误差棒为3次测量结果的标准偏差,后图同此。)
Fig.1 The results of optimization of ascorbic acid mass concentration (The error bar on the dot represents the standard deviation of 3 measurement results. The following pictures are the same.)
图1 抗坏血酸质量浓度条件优化结果 (图中数据点误差棒为3次测量结果的标准偏差,后图同此。)
Fig.1 The results of optimization of ascorbic acid mass concentration (The error bar on the dot represents the standard deviation of 3 measurement results. The following pictures are the same.)
图2 钼酸铵质量浓度条件优化结果 (数据点附近的数字为[H+]/[MoO24-]比值。)
Fig.2 The results of optimization of ammonium molybdate mass concentration (The numbers near the data point represent the ration of [H+] to [MoO24-].)
图2 钼酸铵质量浓度条件优化结果 (数据点附近的数字为[H+]/[MoO24-]比值。)
Fig.2 The results of optimization of ammonium molybdate mass concentration (The numbers near the data point represent the ration of [H+] to [MoO24-].)
图3 酒石酸锑钾质量浓度条件优化结果
Fig.3 The results of optimization of antimony potassium tartrate mass concentration
图3 酒石酸锑钾质量浓度条件优化结果
Fig.3 The results of optimization of antimony potassium tartrate mass concentration
表1 定值方法准确度和可靠性验证结果
Tab.1 The verification results of characterization method accuracy and reliability
| CRM | 批次 | CRM特性值 /(μmol·L-1) | 测量值 /(μmol·L-1) | 误差 /(μmol·L-1) |
|---|---|---|---|---|
| NMIJ7603-a | No.HO135 | 3.10±0.06 | 3.15 | +0.05 |
| NMIJ7602-a | No.MO182 | 1.09±0.06 | 1.12 | +0.03 |
表1 定值方法准确度和可靠性验证结果
Tab.1 The verification results of characterization method accuracy and reliability
| CRM | 批次 | CRM特性值 /(μmol·L-1) | 测量值 /(μmol·L-1) | 误差 /(μmol·L-1) |
|---|---|---|---|---|
| NMIJ7603-a | No.HO135 | 3.10±0.06 | 3.15 | +0.05 |
| NMIJ7602-a | No.MO182 | 1.09±0.06 | 1.12 | +0.03 |
表2 定值方法精密度验证结果
Tab.2 The verification results of characterization method precision
| 序号 | 样品活性磷酸盐浓度测量结果/(μmol·L-1) | |||
|---|---|---|---|---|
| P1批次 | P2批次 | P3批次 | P4批次 | |
| 1 | 0.57 | 1.00 | 2.06 | 4.03 |
| 2 | 0.56 | 1.00 | 2.08 | 4.04 |
| 3 | 0.57 | 1.01 | 2.07 | 4.02 |
| 4 | 0.60 | 1.01 | 2.03 | 4.04 |
| 5 | 0.57 | 1.02 | 2.02 | 4.03 |
| 6 | 0.57 | 1.02 | 1.99 | 4.06 |
| 7 | 0.60 | 1.04 | 2.05 | 4.02 |
| 8 | 0.58 | 1.00 | 2.04 | 4.01 |
| 9 | 0.57 | 1.04 | 2.11 | 4.04 |
| 平均值 | 0.58 | 1.02 | 2.05 | 4.03 |
| RSD/% | 2.45 | 1.57 | 1.72 | 0.37 |
表2 定值方法精密度验证结果
Tab.2 The verification results of characterization method precision
| 序号 | 样品活性磷酸盐浓度测量结果/(μmol·L-1) | |||
|---|---|---|---|---|
| P1批次 | P2批次 | P3批次 | P4批次 | |
| 1 | 0.57 | 1.00 | 2.06 | 4.03 |
| 2 | 0.56 | 1.00 | 2.08 | 4.04 |
| 3 | 0.57 | 1.01 | 2.07 | 4.02 |
| 4 | 0.60 | 1.01 | 2.03 | 4.04 |
| 5 | 0.57 | 1.02 | 2.02 | 4.03 |
| 6 | 0.57 | 1.02 | 1.99 | 4.06 |
| 7 | 0.60 | 1.04 | 2.05 | 4.02 |
| 8 | 0.58 | 1.00 | 2.04 | 4.01 |
| 9 | 0.57 | 1.04 | 2.11 | 4.04 |
| 平均值 | 0.58 | 1.02 | 2.05 | 4.03 |
| RSD/% | 2.45 | 1.57 | 1.72 | 0.37 |
表3 均匀性检验结果
Tab.3 The results of homogeneity test
| 批次 | 实测活性磷酸盐浓度 平均值/(μmol·L-1) | RSD/% | F值 |
|---|---|---|---|
| P1 | 0.57 | 1.89 | 1.37 |
| P2 | 1.02 | 1.34 | 2.20 |
| P3 | 2.05 | 0.91 | 2.01 |
| P4 | 4.02 | 0.62 | 2.20 |
表3 均匀性检验结果
Tab.3 The results of homogeneity test
| 批次 | 实测活性磷酸盐浓度 平均值/(μmol·L-1) | RSD/% | F值 |
|---|---|---|---|
| P1 | 0.57 | 1.89 | 1.37 |
| P2 | 1.02 | 1.34 | 2.20 |
| P3 | 2.05 | 0.91 | 2.01 |
| P4 | 4.02 | 0.62 | 2.20 |
表4 长期稳定性检验结果
Tab.4 The results of long-term stability test
| 批次 | β1 | s(β1) | t95,n-2×s(β1) |
|---|---|---|---|
| P1 | -1.797 7×10-5 | 5.661 8×10-5 | 1.455 6×10-4 |
| P2 | 4.960 5×10-7 | 4.656 0×10-5 | 1.197 1×10-4 |
| P3 | 5.209 6×10-5 | 5.645 7×10-5 | 1.451 5×10-4 |
| P4 | -7.427 9×10-5 | 7.648 5×10-5 | 1.966 4×10-4 |
表4 长期稳定性检验结果
Tab.4 The results of long-term stability test
| 批次 | β1 | s(β1) | t95,n-2×s(β1) |
|---|---|---|---|
| P1 | -1.797 7×10-5 | 5.661 8×10-5 | 1.455 6×10-4 |
| P2 | 4.960 5×10-7 | 4.656 0×10-5 | 1.197 1×10-4 |
| P3 | 5.209 6×10-5 | 5.645 7×10-5 | 1.451 5×10-4 |
| P4 | -7.427 9×10-5 | 7.648 5×10-5 | 1.966 4×10-4 |
图4 长期稳定性检验结果
Fig.4 The results of long-term stability test
图4 长期稳定性检验结果
Fig.4 The results of long-term stability test
图5 短期稳定性检验结果
Fig.5 The results of short-term stability test
图5 短期稳定性检验结果
Fig.5 The results of short-term stability test
表5 短期稳定性检验结果
Tab.5 The results of short-term stability test
| 环境 温度/℃ | 批次 | β1 | s(β1) | t95,n-2×s(β1) |
|---|---|---|---|---|
| -20 | P1 | -3.333 3×10-4 | 2.255 7×10-3 | 9.706 5×10-3 |
| P2 | 5.000 0×10-3 | 2.343 6×10-3 | 1.008 4×10-2 | |
| P3 | 2.333 3×10-3 | 2.934 5×10-3 | 1.262 7×10-2 | |
| P4 | -5.000 0×10-3 | 2.345 9×10-3 | 1.008 4×10-2 | |
| 4 | P1 | -2.333 3×10-3 | 1.536 6×10-3 | 6.611 9×10-3 |
| P2 | -6.000 0×10-3 | 2.335 5×10-3 | 1.005 0×10-2 | |
| P3 | 2.333 3×10-3 | 1.968 8×10-3 | 8.471 8×10-3 | |
| P4 | 4.000 0×10-3 | 3.503 2×10-3 | 1.507 4×10-2 | |
| 25 | P1 | -1.666 7×10-3 | 2.487 3×10-3 | 1.070 3×10-2 |
| P2 | -3.333 3×10-3 | 2.940 9×10-3 | 1.265 5×10-2 | |
| P3 | -1.333 3×10-3 | 3.073 2×10-3 | 1.322 4×10-2 | |
| P4 | -2.333 3×10-3 | 3.805 6×10-3 | 1.637 5×10-2 | |
| 65 | P1 | -1.000 0×10-3 | 1.887 0×10-3 | 8.119 6×10-3 |
| P2 | 0 | 3.107 9×10-3 | 1.337 3×10-2 | |
| P3 | -1.000 0×10-3 | 3.936 0×10-3 | 1.693 7×10-2 | |
| P4 | -3.333 3×10-4 | 3.689 3×10-3 | 1.587 5×10-2 |
表5 短期稳定性检验结果
Tab.5 The results of short-term stability test
| 环境 温度/℃ | 批次 | β1 | s(β1) | t95,n-2×s(β1) |
|---|---|---|---|---|
| -20 | P1 | -3.333 3×10-4 | 2.255 7×10-3 | 9.706 5×10-3 |
| P2 | 5.000 0×10-3 | 2.343 6×10-3 | 1.008 4×10-2 | |
| P3 | 2.333 3×10-3 | 2.934 5×10-3 | 1.262 7×10-2 | |
| P4 | -5.000 0×10-3 | 2.345 9×10-3 | 1.008 4×10-2 | |
| 4 | P1 | -2.333 3×10-3 | 1.536 6×10-3 | 6.611 9×10-3 |
| P2 | -6.000 0×10-3 | 2.335 5×10-3 | 1.005 0×10-2 | |
| P3 | 2.333 3×10-3 | 1.968 8×10-3 | 8.471 8×10-3 | |
| P4 | 4.000 0×10-3 | 3.503 2×10-3 | 1.507 4×10-2 | |
| 25 | P1 | -1.666 7×10-3 | 2.487 3×10-3 | 1.070 3×10-2 |
| P2 | -3.333 3×10-3 | 2.940 9×10-3 | 1.265 5×10-2 | |
| P3 | -1.333 3×10-3 | 3.073 2×10-3 | 1.322 4×10-2 | |
| P4 | -2.333 3×10-3 | 3.805 6×10-3 | 1.637 5×10-2 | |
| 65 | P1 | -1.000 0×10-3 | 1.887 0×10-3 | 8.119 6×10-3 |
| P2 | 0 | 3.107 9×10-3 | 1.337 3×10-2 | |
| P3 | -1.000 0×10-3 | 3.936 0×10-3 | 1.693 7×10-2 | |
| P4 | -3.333 3×10-4 | 3.689 3×10-3 | 1.587 5×10-2 |
表6 原始数据统计检验结果
Tab.6 The results of raw data statistical test
| 批次 | 格拉布 斯检验 | 科克伦 检验 | 狄克逊 检验 | 正态分 布检验 | 总体平均值 /(μmol·L-1) | 总体SD /(μmol·L-1) |
|---|---|---|---|---|---|---|
| P1 | 通过 | 等精度 | 无离群值 | 通过 | 0.53 | 0.03 |
| P2 | 通过 | 等精度 | 无离群值 | 通过 | 1.02 | 0.02 |
| P3 | 通过 | 等精度 | 无离群值 | 通过 | 2.03 | 0.04 |
| P4 | 通过 | 等精度 | 无离群值 | 通过 | 4.01 | 0.04 |
表6 原始数据统计检验结果
Tab.6 The results of raw data statistical test
| 批次 | 格拉布 斯检验 | 科克伦 检验 | 狄克逊 检验 | 正态分 布检验 | 总体平均值 /(μmol·L-1) | 总体SD /(μmol·L-1) |
|---|---|---|---|---|---|---|
| P1 | 通过 | 等精度 | 无离群值 | 通过 | 0.53 | 0.03 |
| P2 | 通过 | 等精度 | 无离群值 | 通过 | 1.02 | 0.02 |
| P3 | 通过 | 等精度 | 无离群值 | 通过 | 2.03 | 0.04 |
| P4 | 通过 | 等精度 | 无离群值 | 通过 | 4.01 | 0.04 |
表7 The results of combine characterization单位:μmol/L
Tab.7
| 实验室 代号 | P1批次 | P2批次 | P3批次 | P4批次 | ||||
|---|---|---|---|---|---|---|---|---|
| 平均值 | SD | 平均值 | SD | 平均值 | SD | 平均值 | SD | |
| A | 0.56 | 0.005 | 1.02 | 0.014 | 2.03 | 0.008 | 4.03 | 0.015 |
| B | 0.49 | 0.008 | 0.98 | 0.008 | 1.98 | 0.008 | 3.96 | 0.019 |
| C | 0.52 | 0.013 | 1.03 | 0.015 | 2.08 | 0.010 | 4.06 | 0.010 |
| D | 0.56 | 0.000 | 1.05 | 0.004 | 2.08 | 0.010 | 4.00 | 0.008 |
| E | 0.50 | 0.009 | 1.02 | 0.009 | 2.00 | 0.008 | 3.98 | 0.027 |
| F | 0.56 | 0.008 | 1.01 | 0.009 | 2.04 | 0.018 | 4.04 | 0.014 |
表7 The results of combine characterization单位:μmol/L
Tab.7
| 实验室 代号 | P1批次 | P2批次 | P3批次 | P4批次 | ||||
|---|---|---|---|---|---|---|---|---|
| 平均值 | SD | 平均值 | SD | 平均值 | SD | 平均值 | SD | |
| A | 0.56 | 0.005 | 1.02 | 0.014 | 2.03 | 0.008 | 4.03 | 0.015 |
| B | 0.49 | 0.008 | 0.98 | 0.008 | 1.98 | 0.008 | 3.96 | 0.019 |
| C | 0.52 | 0.013 | 1.03 | 0.015 | 2.08 | 0.010 | 4.06 | 0.010 |
| D | 0.56 | 0.000 | 1.05 | 0.004 | 2.08 | 0.010 | 4.00 | 0.008 |
| E | 0.50 | 0.009 | 1.02 | 0.009 | 2.00 | 0.008 | 3.98 | 0.027 |
| F | 0.56 | 0.008 | 1.01 | 0.009 | 2.04 | 0.018 | 4.04 | 0.014 |
表8 The results of uncertainty analysis 单位:μmol/L
Tab.8
| 项目 | P1批次 | P2批次 | P3批次 | P4批次 |
|---|---|---|---|---|
| ubb | 0.006 | 0.011 | 0.014 | 0.019 |
| ults | 0.021 | 0.017 | 0.021 | 0.028 |
| uchar | 0.014 | 0.010 | 0.017 | 0.015 |
| uCRM | 0.026 | 0.023 | 0.030 | 0.037 |
| U(k=2) | 0.052 | 0.046 | 0.060 | 0.074 |
| Urel(k=2) | 10% | 5% | 3% | 2% |
表8 The results of uncertainty analysis 单位:μmol/L
Tab.8
| 项目 | P1批次 | P2批次 | P3批次 | P4批次 |
|---|---|---|---|---|
| ubb | 0.006 | 0.011 | 0.014 | 0.019 |
| ults | 0.021 | 0.017 | 0.021 | 0.028 |
| uchar | 0.014 | 0.010 | 0.017 | 0.015 |
| uCRM | 0.026 | 0.023 | 0.030 | 0.037 |
| U(k=2) | 0.052 | 0.046 | 0.060 | 0.074 |
| Urel(k=2) | 10% | 5% | 3% | 2% |
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| [1] | 刘强, 施晓来, 吕海燕, 朱勇, 吴彬. 低盐度海水中重金属标准物质研制[J]. 海洋学研究, 2020, 38(3): 76-82. |
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