Preparation of Certified Reference Materials for Soil Limit Water Content
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摘要:
界限含水率是细粒土定名分类、评价土的工程性质的重要依据，也是黏土矿勘查和工业利用的重要评价指标。不准确的界限含水率测试结果将可能导致严重的工程安全事故，造成人身和经济财产损失。标准物质是保障分析数据准确、可比和有效的重要手段，但当前国内外尚无土壤界限含水率标准物质，可见研制土壤界限含水率标准物质具有重要的现实意义。基于以上原因，本文严格按照《一级标准物质技术规范》(JJF 1006-1994)和《标准物质定值的通用原则及统计学原理》(JJF 1343-2012)等规范和标准，研制了5个土壤界限含水率标准物质(GBW07969、GBW07970、GBW07971、GBW07972、GBW07973)。候选物样品分别采自安徽淮北、山西大同及江苏南京等地，经人工粗碎、烘干、灭菌等加工处理后，采用大型球磨机将候选物样品细碎至粒径小于0.25mm。混匀、分装后每个候选物随机抽取25瓶进行均匀性检验，F实测值均小于临界值F0.05(24，25)=1.96，相对标准偏差(RSD)介于1.16%~2.67%之间，表明均匀性良好。12个月的考察期内进行的5次长期稳定性检验和考虑两种极端环境温度(60℃、-20℃)的短期稳定性检验，均未发现统计学意义的明显变化，候选物样品稳定性良好。经9家实验室采用2种经典土壤界限含水率测试方法联合定值，10mm液限、塑限和塑性指数3个定值指标的标准值分别介于26.3%~39.9%、16.3%~22.2%、10.0%~17.7%之间，梯度系列显著，涵盖了粉质黏土和黏土两种黏性土类别。该系列标准物质可用于仪器设备校准、质量监控、能力验证等技术质量活动，为水工环地质勘查、岩土工程勘察、黏土矿勘查等工作对土壤界限含水率测试数据准确性的要求提供了保障。
Abstract:BACKGROUND Soil limit water content is an important basis for fine-grained soil classification and engineering property evaluation. Additionally, it is an important evaluation index for clay exploration and industrial utilization. Inaccurate test results of soil limit water content may lead to serious engineering safety accidents and personal and economic property losses. Certified reference materials (CRMs) are important for ensuring the accuracy, comparability, and effectiveness of the analyzed data. However, no certified reference materials for soil limit water content exist; therefore, the preparation of CRMs for the soil limit water content holds great significance.
OBJECTIVES To prepare CRMs of soil limit water content.
METHODS In strict accordance with the specifications and standards, such as "Technical Specifications for First-Class Reference Materials" (JJF 1006-1994) and "General Principles and Statistical Principles for the Valuation of Reference Materials" (JJF 1343-2012), five standard materials of soil limit water content (GBW07969, GBW07970, GBW07971, GBW07972, and GBW07973) have been developed. These samples were collected from Huaibei of Anhui province, Datong of Shanxi province, and Nanjing of Jiangsu province. After artificial crushing, drying, and sterilization, the samples were finely crushed to less than 0.25mm by a large ball mill. After particle size analysis, the samples were bottled and numbered in a clean room.
RESULTS Twenty-five bottles of each sample were randomly selected for homogeneity testing. All the measured values of F were less than F0.05 (24, 25)=1.96, and the relative standard deviation (RSD) was between 1.16% and 2.67%, which indicated good uniformity. There were no significant differences in the long-term stability test (12months) and the short-term stability test (60℃, -20℃). The certified values of 10mm liquid limit, plastic limit, and plasticity index were 26.3%-39.9%, 16.9%-22.2%, and 10.0%-17.7%, respectively. The gradient series was significant, which included silty clayey and clayey type of soils.
CONCLUSIONS Five first classes of National CRMs (GBW07969, GBW07970, GBW07971, GBW07972, and GBW07973) of soil limit water content were successfully prepared. This series of CRMs can be used for calibration of instruments and equipment, quality control, capability verification, and other technical quality activities, which provide a guarantee for the accuracy requirements of soil limit water test data in hydraulic environment geological exploration, geotechnical engineering exploration, clay mine exploration, and other related disciplines.
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Key words:
- soil /
- limit water content /
- reference material /
- certified value /
- uncertainty
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表 1 候选物的土质类别、界限含水率指标范围和矿物组成
Table 1. Soil classification, the range of limit water content indexes and mineral compositions of candidates
候选物编号
Codes土质分类
Soil classification界限含水率指标范围
The range of limit water content indexes矿物组成Mineral
compositions10mm液限(%)
10mm liquid limit (%)塑限(%)
Plastic limit (%)塑性指数
Plasticity indexLWC-1 粉土~粉质黏土Silt-Silty clay 25.5~27.5 15.5~17.5 9.0~12.0 石英(55%~60%)，长石(10%)，水云母(10%)，方解石(5%~10%)，绿泥石(10%)，少量沸石Quartz(55%-60%)，Feldspar(10%)，Hydromica(10%)，Calcite(5%-10%)，Chlorite(10%)，Small amount of zeolite LWC-2 粉质黏土Silty clay 28.0~33.0 15.0~19.0 12.0~15.0 石英(55%~60%)，长石(15%~20%)，水云母(10%-15%)，方解石(5%)，绿泥石(5%) Quartz(55%-60%)，Feldspar(15%-20%)，Hydromica(10%-15%)，Calcite(5%)，Chlorite(5%) LWC-3 粉质黏土Silty clay 32.0~35.0 17.0~20.0 13.0~16.0 石英(45%~50%)，长石(10%)，水云母(10%~15%)，蒙脱石(25%~30%)，少量蛭石Quartz (45%-50%)，Feldspar (10%)，Hydromica (10%-15%)，Montmorillonite(25%-30%)，Small amount of vermiculite LWC-4 粉质黏土Silty clay 35.0~38.0 19.0~23.0 14.5~17.0 石英(65%~70%)，长石(10%)，蒙脱石(10%~15%)，水云母(5%) Quartz(65%-70%)，Feldspar(10%)，Montmorillonite(10%-15%)，Hydromica(5%) LWC-5 黏土Clay 39.0~43.0 20.0~24.0 16.0~19.0 石英(70%~75%)，长石(10%)，伊利水云母(5%~10%)，少量蛭石、云母Quartz(70%-75%)，Feldspar(10%)，Illite hydromica (5%-10%)，Small amount of vermiculite and mica 
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表 2 候选物均匀性检验结果
Table 2. Analytical results of the homogeneity tests
候选物编号
Codes检验指标
Test items平均值(%)
Average(%)RSD
(%)F实测值
Fmeasuredubb LWC-1 10mm液限
10mm liquid limit26.4 1.22 1.54 0.15 塑限
Plastic limit16.3 2.67 1.74 0.23 LWC-2 10mm液限10mm liquid limit 31.6 1.16 1.47 0.17 塑限Plastic limit 18.0 2.42 1.36 0.18 LWC-3 10mm液限10mm liquid limit 33.4 1.38 1.58 0.22 塑限Plastic limit 18.7 2.43 1.65 0.23 LWC-4 10mm液限10mm liquid limit 37.1 1.45 1.41 0.23 塑限Plastic limit 21.2 2.46 1.57 0.25 LWC-5 10mm液限10mm liquid limit 39.9 1.26 1.55 0.24 塑限Plastic limit 22.3 2.66 1.47 0.26
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表 3 长期稳定性检验结果
Table 3. Analytical results of the long-term stability tests
候选物编号
Codes检验指标
Test items平均值(%)
Average (%)标准偏差(%)
Standard deviation(%)β1 s(β1) t0.05·s(β1) us长
usLong-termLWC-1 10mm液限
10mm liquid limit26.4 0.13 0.010 0.014 0.043 0.17 塑限
Plastic limit16.3 0.13 -0.005 0.015 0.049 0.19 LWC-2 10mm液限
10mm liquid limit31.4 0.14 0.01 0.016 0.051 0.20 塑限
Plastic limit17.6 0.14 -0.014 0.015 0.048 0.19 LWC-3 10mm液限
10mm liquid limit33.3 0.14 0.003 0.017 0.054 0.21 塑限
Plastic limit18.8 0.15 0.005 0.018 0.057 0.22 LWC-4 10mm液限
10mm liquid limit37.1 0.16 -0.008 0.019 0.059 0.23 塑限
Plastic limit21.0 0.17 0.003 0.02 0.064 0.25 LWC-5 10mm液限
10mm liquid limit39.9 0.18 -0.021 0.017 0.054 0.21 塑限
Plastic limit22.3 0.19 0.013 0.021 0.067 0.26
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表 4 60℃和-20℃下短期稳定性检验结果
Table 4. Analytical results of the short-term stability tests at 60℃ and -20℃
60℃短期稳定性检验Short-term stability tests at 60℃ 候选物编号
Codes检验指标
Test items平均值(%)
Average (%)标准偏差(%)
Standard deviation(%)β1 s(β1) t0.05·s(β1) us短
usShort-termLWC-1 10mm液限
10mm liquid limit26.3 0.05 -0.002 0.007 0.094 0.11 塑限
Plastic limit16.3 0.05 0.003 0.006 0.081 0.09 LWC-2 10mm液限
10mm liquid limit31.7 0.06 0.001 0.009 0.113 0.13 塑限
Plastic limit17.9 0.07 0 0.010 0.131 0.15 LWC-3 10mm液限
10mm liquid limit33.3 0.08 0.001 0.012 0.149 0.17 塑限
Plastic limit18.6 0.10 0.006 0.012 0.157 0.18 LWC-4 10mm液限
10mm liquid limit37.1 0.06 -0.003 0.009 0.110 0.13 塑限
Plastic limit21.0 0.10 -0.001 0.014 0.176 0.20 LWC-5 10mm液限
10mm liquid limit40.1 0.07 0.002 0.010 0.128 0.15 塑限
Plastic limit22.7 0.08 -0.003 0.012 0.149 0.17 -20℃短期稳定性检验Short-term stability tests at -20℃ 候选物编号
Codes检验指标
Test items平均值(%)
Average (%)标准偏差(%)
Standard deviation(%)β1 s(β1) t0.05·s(β1) us短
usShort-termLWC-1 10mm液限
10mm liquid limit26.3 0.06 0 0.009 0.113 0.13 塑限
Plastic limit16.3 0.07 0.002 0.010 0.131 0.15 LWC-2 10mm液限
10mm liquid limit31.7 0.07 0.002 0.010 0.121 0.14 塑限
Plastic limit17.9 0.12 -0.001 0.017 0.210 0.24 LWC-3 10mm液限
10mm liquid limit33.3 0.06 -0.005 0.008 0.097 0.11 塑限
Plastic limit18.6 0.06 -0.001 0.009 0.110 0.13 LWC-4 10mm液限
10mm liquid limit37.0 0.12 -0.011 0.013 0.162 0.18 塑限
Plastic limit20.9 0.16 -0.020 0.011 0.139 0.16 LWC-5 10mm液限
10mm liquid limit40.1 0.08 0.001 0.011 0.141 0.16 塑限
Plastic limit22.5 0.12 -0.001 0.018 0.223 0.25
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表 5 实验室考核数据统计
Table 5. Analytical results of laboratory assessment data
实验室代码
Lab code考核指标
Assessment items平均值(%)
Average(%)标准偏差(%)
Standard deviation (%)A 10mm液限
10mm liquid limit30.8 0.06 塑限
Plastic limit17.8 0.40 B 10mm液限
10mm liquid limit32.0 0.14 塑限
Plastic limit18.4 0.40 C 10mm液限
10mm liquid limit30.8 0.16 塑限
Plastic limit17.2 0.22 D 10mm液限
10mm liquid limit31.4 0.40 塑限
Plastic limit18.3 0.35 E 10mm液限
10mm liquid limit31.5 0.37 塑限
Plastic limit17.6 0.30 F 10mm液限
10mm liquid limit31.9 0.38 塑限
Plastic limit17.7 0.50 G 10mm液限
10mm liquid limit31.4 0.38 塑限
Plastic limit17.4 0.32 H 10mm液限
10mm liquid limit32.1 0.16 塑限
Plastic limit17.9 0.21 I 10mm液限
10mm liquid limit31.7 0.19 塑限
Plastic limit17.9 0.14
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表 6 标准值与扩展不确定度
Table 6. Certified values and expanded uncertainties
定值指标
Certified items单位
UnitsLWC-1 LWC-2 LWC-3 LWC-4 LWC-5 标准值
Certified values不确定度
Uncertainties标准值
Certified values不确定度
Uncertainties标准值
Certified values不确定度
Uncertainties标准值
Certified values不确定度
Uncertainties标准值
Certified values不确定度
Uncertainties10mm液限
10mm liquid limit% 26.3 0.7 31.5 0.8 33.3 0.9 37.0 0.9 39.9 0.9 塑限
Plastic limit% 16.3 0.8 17.8 0.9 18.5 0.9 21.0 1.0 22.2 1.1 塑性指数
Plasticity index/ 10.0 1.0 13.7 1.1 14.8 1.2 16.0 1.3 17.7 1.3
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