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摘要:
海泡石是一种十分重要的非金属矿，被广泛应用于航空、畜牧、化工环保等领域中，贸易活动十分活跃。鉴于中国一直没有海泡石标准物质，国际上的海泡石标准物质定值组分少，为了满足相关研究需求，本文研制了湖南湘潭的海泡石标准物质（GBW07138）。对Ba、Be、Bi、Cd、Ce、Co、Cr、Cs、La、Li、Lu、U、Nb、Nd、Ni、Pb、SiO2、Al2O3、Fe2O3、MgO、CaO、Na2O、K2O、TiO2共24种组分进行均匀性和稳定性检验。针对不同含量、不同性质的组分，采用合理的国家标准方法检验了20种组分的RSD小于3%，其余4种组分Bi、La、Lu、Mo的RSD略大于3%，方差检验的F值均小于列表临界值[F0.05（29，60）=1.65]，表明该标准物质均匀性良好。在稳定性考察期内，24种组分的含量无统计学上的明显变化，表明该标准物质稳定性良好。由9家实验室采用重量法、容量法、X射线荧光光谱法、电感耦合等离子体质谱法等传统化学分析方法和现代仪器分析方法协作定值，最终定值组分63种，涵盖了主量、微量及全部稀土元素，其中海泡石特征组分MgO和烧失量（LOI）的含量分别为18%±0.2%和8.55%±0.19%，这两种组分与现有的标准物质形成一定阶梯性，能够更好地满足海泡石成分分析测试需求。该海泡石标准物质可用于地质找矿、地球化学调查、地质矿产产品测试以及其他行业相关领域样品测试的质量监控标准。而且在研制该标准物质过程中，改良或开发的一些新方法可为后续开发海泡石标准物质提供技术支持。
Abstract:BACKGROUND Sepiolite is a very important non-metallic mineral, which is widely used in aviation, animal husbandry, the chemical industry, environmental protection and other fields. Sepiolite is in great demand and needs a lot of analysis and testing. However, the existing sepiolite reference materials are inadequate and do not satisfy the needs of sepiolite composition analysis. Furthermore, there are no sepiolite reference materials in China, making it necessary to develop one.
OBJECTIVES To prepare a reference material for composition analysis of sepiolite whose certified value components cover as many elements as possible.
METHODS Sepiolite samples were collected from Xiangtan, Hunan Province. The samples were subjected to primary crushing, coarse-grain sieving, inactivation, fine grinding and fine grain sieving. After passing the initial inspection, samples were bottled and numbered. Random samples were taken for homogeneity test, stability test. 24 components were selected for homogeneity and stability test.
RESULTS The results showed that the RSD of 20 components were less than 3%, and the F value of the variance test was less than the critical value of the list[F0.05(29, 60)=1.65], indicating that the homogeneity of the reference material was good. During the investigation period, the contents of 24 components had no significant change, indicating that the standard material was stable. Nine laboratories cooperated with traditional chemical analysis methods and modern instrumental analysis methods to determine the value. The final values were 63 components, covering major, trace and all rare earth elements. The contents of characteristic components MgO and LOI were 18% and 8.55%, respectively. These two components form a certain ladder with the existing reference materials, which can better satisfy the requirements of sepiolite composition analysis.
CONCLUSIONS The developed sepiolite reference material can be used as the quality control standards for geological prospecting, geochemical investigation and testing of geological and mineral products, as well as for other industries to analyze similar materials. Moreover, in the process of developing the reference material, improvements and developments to the new methods will provide technical support for the subsequent development of the sepiolite reference material.
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Key words:
- sepiolite /
- reference material /
- homogeneity test /
- stability test /
- certified values
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表 1 海泡石候选物均匀性检验结果
Table 1. Homogeneity test results of the candidates
统计参数
Statistical parametersBa Be Bi Cd Ce Co Cr Cs 含量测定平均值(×10-6)
Average(×10-6)72.6 3.68 0.18 1.90 37.3 14.2 118 3.96 RSD(%) 1.78 2.27 4.33 2.82 1.28 1.52 1.01 1.43 F实测值
Fmeasure1.10 1.19 1.13 0.95 0.95 1.03 0.93 1.17 Ubb 0.23 0.020 0.002 0.013 0.12 0.022 0.30 0.013 统计参数
Statistical parametersLa Li Lu Mo Nb Nd Ni Pb 含量测定平均值(×10-6)
Average(×10-6)30.4 56.2 0.26 0.22 3.71 23.2 59.8 8.65 RSD(%) 3.72 2.82 4.50 9.49 2.69 1.47 1.51 2.74 F实测值
Fmeasure0.98 1.01 0.83 1.43 1.13 1.06 0.91 1.04 Ubb 0.28 0.089 0.003 0.007 0.021 0.049 0.23 0.027 统计参数
Statistical parametersSiO2 Al2O3 Fe2O3 MgO CaO Na2O K2O TiO2 含量测定平均值(×10-2)
Average(×10-2)63.4 4.46 1.49 18.0 2.58 0.11 0.32 0.18 RSD(%) 0.17 1.04 2.2 0.42 1.77 2.1 1.13 2.59 F实测值
Fmeasure1.03 1.27 1.01 1.19 1.24 0.86 0.55 1.81 Ubb 0.011 0.013 0.002 0.018 0.012 0.001 0.001 0.002 
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表 2 海泡石候选物长期稳定性检验结果
Table 2. Long term stability test results of the candidates
样品
Samples参数
Parameters组分含量(×10-6) Components content (×10-6) Ba Be Bi Cd Ce Co Cr Cs 海泡石
Sepiolite平均值
Average71.9 3.69 0.18 1.95 36.0 14.5 118 3.93 b1 0.2253 0.0137 0.0013 -0.0050 -0.3087 -0.2227 -0.5633 -0.0260 t0.05×s(b1) 3.6349 0.2095 0.0049 0.0513 2.1964 0.44048 2.7345 0.1291 Us 5.72 0.33 0.0077 0.081 3.45 0.69 4.30 0.20 样品
Samples参数
Parameters组分含量(×10-6) Components content (×10-6) La Li Lu Mo Nb Nd Ni Pb 海泡石
Sepiolite平均值
Average30.6 57.7 0.26 0.20 3.85 23.7 58.9 8.68 b1 -0.1137 -0.6933 0.0050 -0.0017 0.1100 -0.2930 -0.4230 0.0633 t0.05×s(b1) 1.2168 2.2426 0.0084 0.0223 0.1812 1.6752 1.7402 0.2533 Us 1.91 3.53 0.013 0.035 0.28 2.63 2.74 0.40 样品
Samples参数
Parameters组分含量(×10-2) Components content (×10-2) K2O TiO2 SiO2 Al2O3 Fe2O3 MgO CaO Na2O 海泡石
Sepiolite平均值
Average63.3 4.44 1.48 18.0 2.57 0.11 0.32 0.18 b1 0.0640 -0.0063 0.0077 -0.0077 0.0027 0.0003 -0.0003 0.0003 t0.05×s(b1) 0.1146 0.0293 0.0113 0.0674 0.02055 0.0032 0.0020 0.0020 Us 0.18 0.046 0.018 0.11 0.032 0.005 0.0032 0.00329
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表 3 海泡石候选物短期稳定性检验结果
Table 3. Short term stability test results of the candidates
温度(℃)
Temperature
(℃)参数
Parameter组分含量Components content (×10-6) Ba Be Bi Cd Ce Co Cr Cs -24℃ 平均值
Average70.9 3.71 0.18 1.66 37.4 14.7 115 3.99 b1 0.39 0.01 0.001 0 0.2 0.04 0.23 0.01 t0.05×s(b1) 0.79 0.06 0.003 0.04 0.21 0.18 0.26 0.06 60℃ 平均值
Average72 3.7 0.18 1.77 35.9 14.9 115 3.94 b1 0.06 0.02 0.001 0 -0.07 0.23 0.2 0.026 t0.05×s(b1) 0.24 0.05 0.003 0.02 0.34 0.31 1.31 0.026 温度(℃)
Temperature
(℃)参数
Parameter组分含量Components content (×10-6) La Li Lu Mo Nb Nd Ni Pb -24℃ 平均值
Average31 57.4 0.25 0.23 3.91 23.8 57.1 8.6 b1 0.12 0.29 0.001 0 0 0.05 0.13 0.016 t0.05×s(b1) 0.16 0.31 0.003 0.01 0.04 0.08 0.37 0.021 60℃ 平均值
Average30.4 58.2 0.26 0.22 3.99 23.2 59.3 8.76 b1 0.06 0.37 0 -0.006 0 0.23 0.36 -0.01 t0.05×s(b1) 0.55 0.63 0.01 0.01 0.02 0.24 0.47 0.07 温度(℃)
Temperature
(℃)参数
Parameter组分含量(×10-2)
Components content (×10-2)SiO2 Al2O3 Fe2O3 MgO CaO Na2O K2O TiO2 -24℃ 平均值Average 63.5 4.42 1.45 18.0 2.55 0.11 0.32 0.19 b1 -0.02 -0.007 0 0.02 -0.001 0 -0.001 0 t0.05×s(b1) 0.03 0.013 0.01 0.04 0.003 0.001 0.003 0.01 60℃ 平均值Average 63.5 4.43 1.46 18.0 2.59 0.12 0.32 0.19 b1 -0.001 0.002 0.001 -0.01 0.001 0.0007 0.001 -0.001 t0.05×s(b1) 0.003 0.005 0.003 0.024 0.01 0.0011 0.003 0.003
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表 4 海泡石候选物分析指标及其分析方法
Table 4. Analytical methods of elements in sepiolite candidates
组分
Component测试方法
Analytical methods组分
Component测试方法
Analytical methodsAg ICP-MS, ES Sb ICP-MS, AFS As ICP-MS, AFS Sc ICP-MS, ICP-OES B ICP-OES, ES Sm ICP-MS, ICP-OES Ba ICP-MS, ICP-OES Sn ICP-MS, ES Be ICP-MS, ICP-OES Sr ICP-MS, ICP-OES Bi ICP-MS, AFS Ta ICP-MS Cd ICP-MS, GFAAS Tb ICP-MS, ICP-OES Ce ICP-MS, ICP-OES Th ICP-MS Co ICP-MS, ICP-OES Tm ICP-MS, ICP-OES Cr ICP-MS, ICP-OES U ICP-MS, LF Cs ICP-MS, ICP-OES V ICP-MS, ICP-OES Cu ICP-MS, ICP-OES W ICP-MS, ICP-OES Dy ICP-MS, ICP-OES Y ICP-MS Er ICP-MS, ICP-OES Yb ICP-MS, ICP-OES Eu ICP-MS, ICP-OES Zn ICP-MS, ICP-OES Ga ICP-MS Zr ICP-MS, ICP-OES Gd ICP-MS, ICP-OES SiO2 GR, VOL, XRF Hf ICP-MS Al2O3 VOL, ICP-OES, XRF Hg CVAAS, AFS Fe2O3 COL, ICP-OES, XRF Ho ICP-MS, ICP-OES FeO VOL In ICP-MS, GFAAS MgO VOL, ICP-OES, XRF La ICP-MS, ICP-OES CaO VOL, ICP-OES, XRF Li ICP-MS, ICP-OES Na2O AAS, ICP-OES, XRF Lu ICP-MS, ICP-OES K2O AAS, ICP-OES, XRF Nb ICP-MS TiO2 COL, ICP-OES, XRF Nd ICP-MS, ICP-OES MnO AAS, ICP-OES, XRF Ni ICP-MS, ICP-OES P2O5 COL, ICP-OES, XRF Pb ICP-MS, ICP-OES H2O+ GR Pr ICP-MS, ICP-OES CO2 VOL, IR Rb ICP-MS, ICP-OES TC VOL, IR S ICP-OES, IR, VOL LOI GR 注：AFS—原子荧光光谱法；GFAAS—石墨炉原子吸收光谱法；CVAAS—冷蒸汽原子吸收光谱法；ES—一米光栅发射光谱法；IR—红外光谱法；VOL—容量法；LF—极谱法；GR—重量法；COL—比色法。
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表 5 海泡石标准物质的认定值及其扩展不确定度
Table 5. Certified values and expanded uncertainty of the sepiolite standard material
组分
Component单位
Unit认定值及扩展不确定度
Certified values and expanded uncertainty组分
Component单位
Unit认定值及扩展不确定度
Certified values and expanded uncertaintyAg 10-6 0.15±0.02 Sb 10-6 (0.57) As 10-6 2.3±0.3 Sc 10-6 5.6±0.5 B 10-6 6.9±0.5 Sm 10-6 4.3±0.5 Ba 10-6 72±7 Sn 10-6 1.2±0.2 Be 10-6 3.6±0.4 Sr 10-6 49±5 Bi 10-6 0.18±0.03 Ta 10-6 0.30±0.04 Cd 10-6 (1.8) Tb 10-6 0.62±0.05 Ce 10-6 39±4 Th 10-6 3.8±0.4 Co 10-6 15±2 Tm 10-6 0.27±0.03 Cr 10-6 116±9 U 10-6 5.3±0.4 Cs 10-6 4.0±0.3 V 10-6 81±7 Cu 10-6 25±2 W 10-6 0.50±0.07 Dy 10-6 3.3±0.3 Y 10-6 23±3 Er 10-6 1.8±0.2 Yb 10-6 1.6±0.2 Eu 10-6 0.8±0.1 Zn 10-6 105±8 Ga 10-6 5.9±0.4 Zr 10-6 43±4 Gd 10-6 4.0±0.6 SiO2 10-2 63.55±0.19 Hf 10-6 (1.2) Al2O3 10-2 4.45±0.07 Hg 10-6 0.16±0.02 TFe2O3 10-2 1.46±0.07 Ho 10-6 0.66±0.05 FeO 10-2 (0.10) In 10-6 0.027±0.003 MgO 10-2 18±0.2 La 10-6 30±4 CaO 10-2 2.56±0.09 Li 10-6 55±5 Na2O 10-2 0.12±0.01 Lu 10-6 0.26±0.02 K2O 10-2 0.32±0.02 Mo 10-6 (0.25) P2O5 10-2 0.41±0.02 Nb 10-6 3.9±0.4 TiO2 10-2 0.18±0.01 Nd 10-6 24±3 MnO 10-2 0.022±0.003 Ni 10-6 57±4 H2O+ 10-2 6.39±0.18 Pb 10-6 8.7±0.7 CO2 10-2 1.63±0.06 Pr 10-6 6.0±0.6 TC 10-2 0.63±0.03 Rb 10-6 20±2 LOI 10-2 8.55±0.19 S 10-6 (136)
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表 6 监控样品质量监控结果
Table 6. Quality control results of the monitoring samples
样品
Samples参数
Parameters组分Components Ag As B Ba Be Bi Cd Ce Co Cr Cs Cu GBW07103 认定值(×10-6)
Certified value(×10-6)0.033 2.1 24 343 12.4 0.53 0.029 108 3.4 3.6 38.4 3.2 平均值(×10-6)
Average(×10-6)0.034 2.13 24.5 322 11.9 0.53 0.031 113 3.60 3.54 39.1 3.45 相对误差(%)
Relative error(%)1.49 0.71 1.03 3.16 2.06 0.00 3.33 2.26 2.86 0.84 0.90 3.76 GBW07121 认定值(×10-6)
Certified value(×10-6)0.027 0.25 15 1140 1.7 0.094 0.06 48 7.5 23 2.6 2.6 平均值(×10-6)
Average(×10-6)0.025 0.26 15.3 1210 1.64 0.10 0.055 46.3 7.21 22.5 2.54 2.63 相对误差(%)
Relative error(%)3.85 1.96 0.99 2.98 1.80 3.59 4.35 1.80 1.97 1.10 1.17 0.57 样品
Samples参数
Parameters组分Components Dy Er Eu Ga Gd Hf Hg* Ho In La Li Lu GBW07103 认定值(×10-6)
Certified value(×10-6)10.2 6.5 0.85 19 9.3 6.3 4.3 2.05 0.02 54 131 1.15 平均值(×10-6)
Average(×10-6)10.5 6.50 0.86 19.5 9.05 6.11 4.24 2.12 0.021 55.9 137 1.16 相对误差(%)
Relative error(%)2.94 0.00 1.18 2.63 2.69 3.02 1.40 3.41 5.00 3.52 4.58 0.87 GBW07121 认定值(×10-6)
Certified value(×10-6)1.52 0.76 1 18.2 2.4 3.3 4 0.27 0.03 25 24.7 0.11 平均值(×10-6)
Average(×10-6)1.52 0.76 1.01 17.7 2.32 3.26 3.89 0.27 0.031 24.4 23.9 0.11 相对误差(%)
Relative error(%)0.00 0.00 1.00 2.75 3.33 1.21 2.75 0.00 3.33 2.40 3.24 0.00 样品
Samples参数
Parameters组分Components Mo Nb Nd Ni Pb Pr Rb S Sb Sc Sm Sn GBW07103 认定值(×10-6)
Certified value(×10-6)3.5 40 47 2.3 31 12.7 466 380 0.21 6.1 9.7 12.5 平均值(×10-6)
Average(×10-6)3.44 41.2 47.0 2.40 32.0 13.0 474 369 0.22 6.25 10.0 12.3 相对误差(%)
Relative error(%)1.71 3.00 0.00 4.35 3.23 2.36 1.72 2.89 4.76 2.46 3.09 1.60 GBW07121 认定值(×10-6)
Certified value(×10-6)0.27 4.5 21 13 7.6 5.7 57 50 0.063 5 3.3 0.8 平均值(×10-6)
Average(×10-6)0.28 4.43 20.5 13.5 7.45 5.62 55.0 52.0 0.066 5.03 3.22 0.85 相对误差(%)
Relative error(%)3.70 1.56 2.38 3.85 1.97 1.40 3.51 4.00 4.76 0.60 2.42 6.25 样品
Samples参数
Parameters组分Components Sr Ta Tb Th Tm U V W Y Yb Zn Zr GBW07103 认定值(×10-6)
Certified values(×10-6)106 7.2 1.65 54 1.06 18.8 24 8.4 62 7.4 28 167 平均值(×10-6)
Average(×10-6)110 7.31 1.71 55.5 1.11 18.3 23.3 8.22 62.6 7.51 31.0 156 相对误差(%)
Relative error(%)3.77 1.53 3.64 2.78 4.72 2.66 2.92 2.14 0.97 1.49 10.71 6.59 GBW07121 认定值(×10-6)
Certified value(×10-6)690 0.34 0.29 1.9 0.11 0.4 45 0.42 7.3 0.69 46 90 平均值(×10-6)
Average(×10-6)679 0.33 0.30 1.85 0.11 0.39 46.6 0.44 6.93 0.71 40.6 101 相对误差(%)
Relative error(%)1.59 2.94 3.45 2.63 0.00 2.50 3.56 4.76 5.07 2.90 11.74 12.22 样品
Samples参数
Parameters组分Components SiO2 Al2O3 Fe2O3 FeO MgO CaO Na2O K2O P2O5 TiO2 MnO H2O+ CO2 LOI GBW07103 认定值(×10-2)
Certified value(×10-2)72.83 13.4 1 1.03 0.42 1.55 3.13 5.01 0.093 0.29 0.06 0.61 0.15 0.69 平均值(×10-2)
Average(×10-2)72.8 13.3 0.97 1.06 0.45 1.53 3.11 5.11 0.095 0.30 0.058 0.62 0.14 0.67 相对误差(%)
Relative error(%)0.04 0.75 3.00 2.91 7.14 1.29 0.64 2.00 2.15 3.45 3.33 1.64 6.67 2.90 GBW07121 认定值(×10-2)
Certified value(×10-2)66.3 16.3 1.34 1.6 1.63 2.66 5.3 2.6 0.131 0.297 0.056 - 0.35 1.28 平均值(×10-2)
Average(×10-2)66.4 16.2 1.37 1.55 1.61 2.69 5.22 2.56 0.13 0.28 0.054 - 0.33 1.23 相对误差(%)
Relative error(%)0.15 0.61 2.24 3.13 1.23 1.13 1.51 1.54 0.76 5.72 3.57 - 5.71 3.91 注：“*”代表组分(Hg)含量单位为10-9。
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| 引用本文: |
魏双, 王家松, 徐铁民, 方蓬达, 王力强, 王娜. 海泡石化学成分分析标准物质研制[J]. 岩矿测试, 2021, 40(5): 763-773. doi: 10.15898/j.cnki.11-2131/td.202102090022
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| Citation: |
WEI Shuang, WANG Jia-song, XU Tie-min, FANG Peng-da, WANG Li-qiang, WANG Na. Preparation of Sepiolite Reference Material for Chemical Composition Analysis[J]. Rock and Mineral Analysis, 2021, 40(5): 763-773. doi: 10.15898/j.cnki.11-2131/td.202102090022
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