石煤钒矿成分分析标准物质的研制

田宗平; 彭君; 王干珍; 易晓明; 曹健; 秦毅

doi:10.15898/j.cnki.11-2131/td.202001070008

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F_0.05(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:

BACKGROUNDThe 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.

OBJECTIVESTo prepare standard materials for composition analysis of stone coal vanadium ore.

METHODSOre 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.

RESULTSFor the uniformity test of randomly selected 4×35 bottles, the measured values of F were all less than F_0.05(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.

CONCLUSIONSThe 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.

石煤钒矿成分分析标准物质的研制

Preparation of Standard Materials for Composition Analysis of Stone Coal Vanadium Ore