Journal of Marine Sciences ›› 2023, Vol. 41 ›› Issue (3): 92-100.DOI: 10.3969/j.issn.1001-909X.2023.03.009
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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
CLC Number:
Cite this article
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.
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URL: http://hyxyj.sio.org.cn/EN/10.3969/j.issn.1001-909X.2023.03.009
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.)
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.)
Fig.2 The results of optimization of ammonium molybdate mass concentration (The numbers near the data point represent the ration of [H+] to [MoO24-].)
Fig.2 The results of optimization of ammonium molybdate mass concentration (The numbers near the data point represent the ration of [H+] to [MoO24-].)
Fig.3 The results of optimization of antimony potassium tartrate mass concentration
Fig.3 The results of optimization of antimony potassium tartrate mass concentration
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 |
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 |
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 |
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 |
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 |
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 |
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 |
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 |
Fig.4 The results of long-term stability test
Fig.4 The results of long-term stability test
Fig.5 The results of short-term stability test
Fig.5 The results of short-term stability test
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 |
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 |
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 |
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 |
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 |
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 |
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% |
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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