Preparation of Standard Materials for Composition Analysis of Stone Coal Vanadium Ore
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摘要:
石煤钒矿资源的开发和合理利用需要对其成分进行准确的分析测试和质量控制。目前，国内外尚未有石煤钒矿成分分析的标准物质，现有钒成分分析标准物质无论是其五氧化二钒含量，还是定值成分都无法满足我国对石煤钒矿勘查、开发和研究需要。本文对采自湖北省崇阳县小源冲钒矿、湖南省芷江县牛牯坪钒矿、湖南省古丈县岩头寨钒矿和湖南省凤凰县黑冲钒矿等4个大型石煤钒矿区样品开展了标准物质研制工作，研制了4个石煤钒矿成分分析标准物质(GBW07875、GBW07876、GBW07877、GBW07878)。将矿层样品、顶底板岩石和人工剥离高品位样品，经过颚式初碎、对辊中碎、粗粒过筛混匀、配矿混匀、盘式细磨、细粒过筛、灭活混匀等加工处理，经初检合格后，装瓶和编号。随机抽取的4×35瓶样品进行均匀性检验，F实测值均小于F0.05(34，70)=1.60，且相对标准偏差(RSD)在0.31%~7.48%之间，表明样品的均匀性好。对随机抽取样品进行长期稳定性检验和短期稳定性检验，结果没有发现统计学意义的明显差异，表明样品的稳定性良好。通过9家实验室参加协作定值研究，定值成分包括V2O5、C和SiO2等共16种成分，其中4个石煤钒矿成分分析标准物质中的V2O5的质量分数分别为0.63%、0.86%、1.55%、3.99%，涵盖边界品位0.50%、工业品位0.70%、富矿品位≥1%，碳含量分别为2.40%、3.46%、5.60%、7.27%。本批次4个标准物质的研制成功，可为石煤钒矿的科学利用和研究提供参考和借鉴。
Abstract:BACKGROUND The development and rational utilization of stone coal vanadium ore resources require accurate analysis of its components and quality control. At present, there is no standard material for composition analysis of vanadium ore in the world, and the existing standard material cannot meet the needs of exploration, development and research of vanadium ore in China, either in the content of vanadium pentoxide or in the certified values of other elements.
OBJECTIVES To prepare standard materials for composition analysis of stone coal vanadium ore.
METHODS Ore samples, roof and floor rocks and artificially stripped high-grade samples were collected from four large stone coal vanadium districts, including Xiaoyuanchong vanadium mine in Chongyang County, Hubei Province, the Niuguuping in Zhijiang County, Hunan Province, the Yantouzhai in Guzhang County, Hunan Province, and the Heichong in Fenghuang County, Hunan Province. The samples were subjected to jaw-type primary crushing, roller crushing, coarse-grain sieving and mixing, ore blending and mixing, disc fine grinding, fine-grain sieving, and inactivation. After passing the initial inspection, samples were bottled and numbered.
RESULTS For the uniformity test of randomly selected 4×35 bottles, the measured values of F were all less than F0.05(34, 70)=1.60, and the relative standard deviation was between 0.31% and 7.48%, indicating good uniformity of the samples. Long-term and short-term stability tests were carried out on randomly selected samples, and no statistically significant difference was found, indicating good stability of the samples. Nine laboratories participated in the collaborative certified value research, which included 16 components such as V2O5, C and SiO2. Mass fractions of V2O5 in the four stone coal vanadium ore standard materials were 0.63%, 0.86%, 1.55%, 3.99%, covering cut-off grade of 0.50%, industrial grade of 0.70%, and rich-ore grade of ≥ 1%. Carbon contents of four standard materials were 2.40%, 3.46%, 5.60% and 7.27%, respectively.
CONCLUSIONS The successful development of 4 standard substances (GBW07875, GBW07876, GBW07877, GBW07878) in this batch can provide reference for scientific utilization and research of stone coal vanadium ore.
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Key words:
- stone coal vanadium ore /
- reference materials /
- component analysis /
- certified values
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表 1 候选物的采集与制备
Table 1. Collection and preparation of candidates
候选物编号 矿区名称 候选物样品采集与制备 标准物质样品配制与制备 样品
编号描述 粒度
(mm)质量
(kg)五氧化二钒
含量(%)分取质量
(kg)总质量
(kg)粒度
(mm)五氧化二钒
含量(%)分装数
(瓶)GV-1 HB-XYC Y-1 矿层样 1.0 175 0.70 180 240 0.097 0.62 1599 Y-2 顶底板样 1.0 160 0.35 60 GV-2 HN-NGP Y-3 矿层样 1.0 260 0.91 210 240 0.097 0.87 1391 Y-4 顶底板样 1.0 90 0.52 30 GV-3 HN-YTZ Y-5 矿层样 1.0 195 1.01 165 245 0.097 1.55 1511 Y-6 顶底板样 1.0 95 0.50 15 Y-7 富矿样 1.0 75 3.16 65 GV-4 HN-HC Y-8 人工剥离
富矿样1.0 325 3.98 240 240 0.097 4.01 1646 
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表 2 候选物均匀性检验结果统计分析
Table 2. Statistical analysis of homogeneity test for the candidates
候选物
编号统计项目 成分含量 V2O5 SiO2 Al2O3 Fe2O3 P S C GV-1 $\bar x $ (%)0.64 81.05 7.20 1.35 0.071 0.24 2.39 RSD(%) 3.57 0.31 1.10 1.57 2.79 6.49 4.28 F实测值 1.41 0.81 1.28 0.86 0.63 1.19 1.04 GV-2 $\bar x $ (%)0.86 77.41 7.58 1.66 0.096 0.328 3.50 RSD(%) 2.46 0.43 1.65 2.04 2.86 5.89 7.48 F实测值 0.98 0.68 0.72 0.77 1.16 1.20 0.70 GV-3 $\bar x $ (%)1.55 76.89 5.36 1.97 0.17 0.46 5.62 RSD(%) 1.70 0.28 1.83 1.68 3.29 2.78 3.02 F实测值 0.82 1.06 0.85 1.59 1.24 0.79 0.76 GV-4 $\bar x $ (%)3.97 63.87 8.48 2.00 0.26 0.53 7.31 RSD(%) 1.43 0.28 1.58 2.54 1.37 5.67 5.33 F实测值 0.65 0.76 0.65 0.70 1.10 1.10 0.88 候选物
编号统计项目 成分含量 Cu Pb Zn Ni Cd Mo As Ag U x(×10-6) 65.8 23.5 45.8 30.1 1.38 63.8 29.7 4.39 36.2 GV-1 RSD(%) 2.02 5.67 3.25 1.64 3.35 2.34 5.38 2.23 3.38 F实测值 1.24 0.87 0.43 0.77 1.02 0.77 1.10 0.65 1.19 x(×10-6) 91.1 25.7 86.5 42.7 2.66 67.0 53.8 6.62 30.2 GV-2 RSD(%) 1.51 6.26 3.69 3.01 1.88 2.81 4.35 2.42 3.08 F实测值 1.00 0.58 0.69 0.65 1.36 1.58 1.01 0.73 1.27 x(×10-6) 187.2 44.2 130.7 56.4 8.03 49.0 71.7 11.98 39.5 GV-3 RSD(%) 2.13 5.68 1.70 1.87 2.22 2.65 3.71 2.99 3.37 F实测值 0.82 0.94 0.96 1.18 0.87 0.98 1.03 0.72 0.91 $\bar x $ (×10-6)335.2 69.31 331.3 107.8 38.18 103.8 130.1 12.63 58.98 GV-4 RSD(%) 1.95 4.26 1.48 1.61 2.60 2.39 3.84 1.96 3.19 F实测值 1.58 1.29 1.18 1.10 0.71 1.19 1.30 1.53 0.62
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表 3 候选物稳定性检验结果统计分析
Table 3. Statistical analysis of stability test for the candidates
样品编号 统计项目 成分含量 V2O5 SiO2 Al2O3 Fe2O3 P S C GV-1 $\bar x $ (%)0.63 80.83 7.18 1.36 0.070 0.26 2.58 RSD(%) 0.52 0.13 0.59 2.30 1.34 2.54 0.71 b1 -0.00020 0.0013 0.0057 0.0029 0.00014 -0.00014 -0.0013 t0.05×s(b1) 0.0012 0.041 0.012 0.011 0.00024 0.0025 0.0065 GV-2 $\bar x $ (%)0.86 77.74 7.58 1.68 0.10 0.34 3.68 RSD(%) 0.75 0.090 1.22 1.97 1.57 2.49 2.32 b1 0.00049 -0.0042 0.0076 0.0027 0.000010 0.00021 0.00062 t0.05×s(b1) 0.0023 0.025 0.032 0.012 0.00058 0.0032 0.033 GV-3 $\bar x $ (%)1.56 76.77 5.36 1.95 0.17 0.47 5.73 RSD(%) 0.78 0.18 0.56 1.51 1.45 2.92 0.39 b1 0.0011 -0.007 0.0028 0.0029 0.00029 0.0000 -0.0036 t0.05×s(b1) 0.0041 0.051 0.010 0.010 0.0008 0.0053 0.0052 GV-4 $\bar x $ (%)4.03 63.71 8.54 2.03 0.26 0.55 7.30 RSD(%) 0.23 0.22 0.12 0.59 0.88 2.51 0.25 b1 0.00088 -0.014 -0.00009 0.0011 0.00017 -0.00029 0.00073 t0.05×s(b1) 0.0032 0.047 0.0040 0.0041 0.00080 0.0052 0.0069 样品编号 统计项目 成分含量 Cu Pb Zn Ni Cd Mo As Ag U GV-1 $\bar x $ (×10-6)67.80 26.48 45.37 29.70 1.43 62.86 33.45 4.54 37.39 RSD(%) 0.44 4.73 3.97 2.57 6.00 2.34 2.03 1.82 0.80 b1 0.016 -0.075 -0.14 0.060 -0.0095 0.13 -0.11 -0.0044 0.017 t0.05×s(b1) 0.11 0.46 0.64 0.27 0.028 0.51 0.16 0.030 0.11 GV-2 $\bar x $ (×10-6)93.25 28.11 88.39 41.65 2.76 66.46 58.51 6.85 31.13 RSD(%) 1.61 2.00 3.25 2.35 3.08 1.89 3.11 1.61 0.39 b1 0.12 -0.060 -0.31 0.077 -0.0076 0.098 -0.30 0.0014 -0.0060 t0.05×s(b1) 0.53 0.18 0.94 0.34 0.029 0.44 0.41 0.042 0.045 GV-3 $\bar x $ (×10-6)192.4 43.07 127.2 55.92 8.36 48.17 75.00 12.18 40.35 RSD(%) 1.43 2.61 2.39 2.47 0.91 2.11 3.64 0.37 0.51 b1 0.20 0.067 -0.31 0.12 -0.0045 0.081 -0.39 0.0032 -0.016 t0.05×s(b1) 0.98 0.41 1.00 0.48 0.028 0.36 0.75 0.016 0.07 GV-4 $\bar x $ (×10-6)336.5 68.41 331.2 107.6 39.92 102.3 132.7 13.00 58.56 RSD(%) 1.34 2.23 2.05 1.37 1.72 0.89 3.85 1.01 0.54 b1 0.49 0.18 -0.62 0.12 -0.051 0.066 -0.58 0.00077 -0.023 t0.05×s(b1) 1.46 0.48 2.31 0.51 0.24 0.32 1.63 0.050 0.11 注：表中 $\bar x $ 为成分测定的平均值，s为标准偏差，b1为回归系数。
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表 4 石煤钒矿成分分析标准物质各成分定值方法
Table 4. Determination methods of each parameter of standard materials for composition analysis of stone coal vanadium ore
成分 数据组数 分析测试方法 成分 数据组数 分析测试方法 V2O5 9 VOL，COL，ICP-OES SiO2 9 GR，ICP-OES，XRF Al2O3 9 VOL，ICP-OES，XRF Fe2O3 9 VOL，COL，ICP-OES，XRF，FAAS P 9 COL，ICP-OES，XRF S 9 VOL，HCS C 9 GC，VOL，HCS Cu 9 ICP-OES，ICP-MS，XRF Pb 9 ICP-OES，ICP-MS Zn 9 ICP-OES，ICP-MS Ni 9 ICP-OES，ICP-MS，XRF Cd 9 ICP-MS Mo 9 ICP-OES，ICP-MS，POL，COL As 9 AFS Ag 9 FAAS U 9 ICP-MS 注：VOL—容量法；COL—分光光度法；ICP-OES—电感耦合等离子体发射光谱法；GR—重量法；XRF—X射线荧光光谱法；FAAS—火焰原子吸收光谱法；GC—元素分析仪法；HCS—高频燃烧-红外吸收光谱法；ICP-MS—电感耦合等离子体质谱法；POL—极谱法；AFS—原子荧光光谱法。
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表 5 石煤钒矿成分分析标准物质的标准值和不确定度
Table 5. Standard values and uncertainties of standard materials for composition analysis of stone coal vanadium ore
成分 质量分数(×10-2) GV-1 GV-2 GV-3 GV-4 V2O5* 0.62±0.03 0.86±0.03 1.55±0.03 3.99±0.08 SiO2* 80.72±0.19 77.71±0.29 76.75±0.24 63.84±0.34 Al2O3* 7.00±0.16 7.52±0.21 5.37±0.13 8.49±0.13 Fe2O3* 1.31±0.07 1.66±0.08 1.93±0.07 2.00±0.05 P 0.067±0.002 0.094±0.004 0.16±0.01 0.25±0.01 S 0.26±0.02 0.34±0.03 0.49±0.03 0.58±0.04 C 2.40±0.10 3.46±0.20 5.60±0.13 7.27±0.24 成分 质量分数(×10-6) GV-1 GV-2 GV-3 GV-4 Cu 70±3 93±4 185±8 333±14 Pb 29±4 27±3 43±3 71±8 Zn 49±5 88±7 129±7 334±15 Ni 30±2 41±3 55±3 104±4 Cd 1.4±0.2 2.6±0.2 8.3±0.3 39±2 Mo 63±4 67±4 48±3 100±4 As 32±3 54±4 71±6 125±11 Ag 4.5±0.3 6.5±0.4 11.6±0.7 12.7±0.7 U 40±2 33±2 43±3 61±4 注：“*”表示总量(以氧化物计)。
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表 6 国家一级标准物质实测结果与标准值对比
Table 6. Comparison of certified results and certified results of national standard materials
标准物质编号 成分 计量单位 标准值 实测值 标准物质编号 成分 计量单位 标准值 实测值 GBW07226 V2O5 10-2 0.572±0.009 0.562 GBW07103 SiO2 10-2 72.83±0.10 72.79 GBW07103 Al2O3 10-2 13.40±0.07 13.41 GBW07108 Fe2O3 10-2 2.52±0.07 2.48 GBW07105 P 10-2 0.413±0.013 0.411 GBW07233 S 10-2 0.72±0.03 0.73 GBW07108 C 10-2 9.0±0.2 8.92 GBW07406 Cu 10-6 390±14 389 GBW07318 Pb 10-6 66±6 66.5 GBW07311 Zn 10-6 373±14 365 GBW07105 Ni 10-6 140±7 141 GBW07162 Cd 10-6 32±2 32.2 GBW07164 Mo 10-6 137±17 146 GBW07164 As 10-6 260±30 251 GBW07237 Ag 10-6 13.5±0.8 13.2 GBW04108 U 10-6 79(s=0.0002) 81
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