GBW10010a大米标准物质复(研)制及数据特征

杨榕; 顾铁新; 潘含江; 刘妹; 周国华

doi:10.15898/j.cnki.11-2131/td.202005210073

GBW10010a大米标准物质复(研)制及数据特征

中国地质科学院地球物理地球化学勘查研究所, 河北廊坊 065000

基金项目:
中国地质科学院基本科研业务费项目“南极玄武岩、锂辉石及黝铜矿等36种地质标准物质研制”（YYWF201622）

详细信息

作者简介: 杨榕, 硕士研究生, 工程师, 地球化学专业。E-mail:yangrong0516@163.com

通讯作者: 顾铁新, 教授级高级工程师, 地球化学专业。E-mail:gutiexin@163.com

中图分类号: TQ421.31

收稿日期: 2020-04-09

修回日期: 2020-08-03

录用日期: 2020-09-19

Preparation of Reference Materials GBW10010a for Rice Component and Data Characteristics

Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Science, Langfang 065000, China

More Information

Corresponding author: Tie-xin GU, gutiexin@163.com

Received Date: 09 April 2020

Revised Date: 03 August 2020

Accepted Date: 19 September 2020

摘要

摘要: 随着我国对生态文明建设的重视，自然资源综合调查势在必行，对生物标准物质亦提出了新的需求。当前相关调研工作已经大面积开展，自然资源综合调查、农产品与食品安全评价都需要对生物样品元素组成进行准确测试，需要以生物标准物质作为生物成分测试量值比对和溯源的基础，因此对生物基体标准物质的需求量大幅增加。大米作为主要粮食之一，其食品安全日益受到重视，对大米中的化学成分进行准确的分析测试具有重要的现实意义，因而对大米标准物质的需求量尤为突出，但目前大米成分分析标准物质已供不应求。本文严格按照《标准物质定值的通用原则及统计学原理》（JJF 1343—2012）和《地质分析标准物质的研制》（JJF 1646—2017）等相关规范要求，开展了GBW10010a大米成分分析标准物质的复（研）制工作，包括样品采集、加工制备、均匀性检验、稳定性检验、多家实验室协作定值测试及不确定度评定等关键环节。结果表明：本次复（研）制的大米标准物质定值成分多样、量值准确可靠，符合国家一级标准物质的要求。GBW10010a共定值54项主微量元素，包括Ag、Al、As、B、Ba、Be、Bi、Ca、Cd、Ce、Co、Cr、Cs、Cu、Dy、Er、Eu、Fe、Gd、Ge、Hg、Ho、K、La、Li、Ho、Mg、Mn、Mo、N、Na、Nb、Nd、Ni、P、Pb、Pr、Rb、S、Sb、Sc、Se、Si、Sm、Sr、Tb、Th、Tl、Tm、U、V、Y、Yb、Zn，其中的39项元素给出了标准值及不确定度，包括Ag、Al、As、B、Ba、Ca、Cd、Ce、Co、Cs、Cu、Dy、Er、Fe、Hg、K、Li、Mg、Mn、Mo、N、Na、Nd、Ni、P、Pb、Pr、Rb、S、Sb、Se、Si、Sm、Sr、Tb、Tl、Y、Yb、Zn；15项元素提供参考值，包括Be、Bi、Cr、Eu、Gd、Ge、Ho、Ho、La、Nb、Sc、Th、Tm、U、V。与原有GBW10010大米标准物质相比较，GBW10010a中As、Cd、Co、Cr、Cu、Hg、Mn、Mo、Ni、Zn等重金属元素含量显著下降，其中Cd、Cu、Zn降幅较大，分别下降约39%、43%、38.7%，一定程度上反映了农田生态环境的改善。本批标准物质定值元素总数量增加了6项，新增定值元素Ag、Nb（Nb给出参考值），并且各项元素不确定度范围整体上有所缩小，如Al、Cd、Cu、Fe、K、Mg、Mo、Na、P、Pb、Se、Zn等对生物易有影响的重要元素，表明了地质分析测试方法技术的进步及定值水平的提高。本批标准物质定值元素涵盖了具有生物效应的大部分主微量元素，适用于农业生态环境地球化学调查与评价、生物样品测试、农产品质量与食品安全评价样品测试时的分析仪器校正、分析方法评价和分析质量监控等多个领域。
- 标准物质 /
- 大米 /
- 复(研)制 /
- 均匀性检验 /
- 稳定性检验 /
- 定值元素 /
- 质量监控
Abstract: BACKGROUNDWith the increased attention paid for the construction of ecological civilization, a comprehensive survey of natural resources is imperative, and new requirements for biological reference materials have also been put forward. At present, relevant research work has been widely carried out. The comprehensive investigation of natural resources, agricultural products and food safety evaluation all need to accurately test the element composition of biological samples, and biological reference materials are needed as the basis for the comparison and traceability of biological components. The demand for biological matrix reference materials has increased significantly. As one of the main foods, the food safety of rice has been paid more and more attention. It is of great practical significance to carry out accurate analysis of the chemical components in rice. Therefore, the demand for rice is particularly prominent, but the rice reference materials for composition analysis are still lacking. OBJECTIVESTo develop rice certified reference material (GBW10010a) and compare it with the data characteristics of GBW10010. METHODSThe rice certified reference material (GBW10010a) was prepared in strict accordance with relevant specifications. The collected candidates were prepared through coarse crushing, drying, fine crushing, sieving, blending and other steps. The particle size distribution was detected by BT-9000ST laser particle size analyzer. 15 bottle samples were randomly selected and homogeneity testing was carried out by ICP-MS and ICP-OES, etc. The data were statistically calculated by one-way ANOVA, indicating good homogeneity of the samples. The long-term stability of the standard material under the specified storage conditions was investigated. The linear model was used to evaluate the stability of the sample. The determination of 60 components was carried out by means of ICP-MS, ICP-OES, AFS, COL, VOL, XRF, IC and other Analytical test methods. RESULTSThe rice reference material prepared in this research has diverse fixed value components, accurate and reliable measurement values, and meet the requirements of national first-level reference material. GBW10010a has a total of 54 main trace elements. 39 elements have certified values and uncertainties and 15 elements only have reference values. The content of heavy metal elements such as As, Cd, Co, Cr, Cu, Hg, Mn, Mo, Ni, Zn in GBW10010a decreased significantly, among which Cd, Cu, and Zn decreased by about 39%, 43% and 38.7%, respectively. CONCLUSIONSTo a certain extent, the values reflects the improvement of farmland ecological environment. Compared with the original GBW10010, the total number of certified value elements has increased by 6 items, including Ag and Nb (Nb gives reference values). Moreover, the uncertainty of each element is reduced, including biological-related elements Al, Cd, Cu, Fe, K, Mg, Mo, Na, P, Pb, Se, and Zn. The reduction indicates the technological advancement of the geological analysis and the improvement of the certified value level. In addition, the content of heavy metal elements in GBW10010a decreased significantly, reflecting the improvement of farmland ecological environment. The designated elements of the reference materials cover most of the main and trace elements with biological effects, and are suitable for the calibration of analytical instruments, evaluation of analytical methods, and monitoring analytical quality during agricultural ecological environment geochemical surveys and evaluation, biological sample analysis, agricultural product quality and food safety evaluation.
- certified reference material /
- rice /
- remanufacturing /
- homogeneity test /
- stability test /
- certified value element /
- quality monitoring

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图 1 候选物样品加工制备流程示意图

Figure 1.

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图 2 GBW10010a粒径分布曲线

Figure 2.

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图 3 GBW10010与GBW10010a重金属含量对比

Figure 3.

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表 1 GBW10010a候选物粒度分布统计

Table 1. Statistics of particle size distribution for GBW10010a candidate material

粒径(μm)	区间含量(%)	累计含量(%)
＜10	29.87	29.87
10~12	5.68	35.55
12~14	5.07	40.62
14~17	6.84	47.46
17~20	6.14	53.6
20~25	8.78	62.38
25~30	7.14	69.52
30~35	5.8	75.32
35~40	4.83	80.15
40~45	4.07	84.22
45~50	3.5	87.72
50~63	6.82	94.54
63~75	3.39	98.0
75~100	1.87	99.8
100~120	0.2	100
120~140	0	100
140~ 170	0	100
170~200	0	100
200~250	0	100
250~300	0	100

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表 2 GBW10010a候选物均匀性检验结果

Table 2. Homogeneity test results for GBW10010a candidate material

元素	X	RSD (%)	F	U_bb
Al	150	4.53	0.83	3.03
As	0.078	6.9	0.97	0.00
B	0.688	9.61	1.30	0.02
Ba	0.146	8.27	1.66	0.01
Be	0.738	6.25	1.07	0.01
Bi	1.42	24.97	1.23	0.11
Ca	73.6	2.37	1.50	0.78
Cd	53.56	3.84	1.14	0.53
Co	6.46	9.43	1.25	0.20
Cr	0.073	12.87	1.16	0.00
Cs	3.12	9.14	1.28	0.10
Cu	2.98	3.08	1.34	0.03
Fe	4.02	3.3	1.12	0.03
Ge	1.82	14.72	2.30	0.17
K	914	1.78	1.16	4.38
Li	16.6	10.72	1.21	0.55
Mg	130	2.65	1.19	1.02
Mn	10.9	4.64	1.02	0.05
Mo	0.422	4.07	1.46	0.01
Na	11.8	14.18	1.06	0.28
Ni	0.302	3.18	2.09	0.01
P	781	4.71	1.29	13.05
Pb	0.098	23.85	1.09	0.00
Rb	1.75	3.01	1.55	0.02
S	1037	5.33	0.96	23.87
Sb	8.49	23.82	1.15	0.54
Si	48.6	15.28	1.20	2.27
Ti	2.17	1.8	2.24	0.02
Y	209	8.29	2.15	10.52
Yb	0.193	12.79	1.25	0.01
Zn	13.5	0.78	1.34	0.04
注：X为计算平均值; RSD为相对标准偏差; F检验临界值F_0.05(14，15)=2.42;U_bb为均匀性引入的不确定度。

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表 3 GBW10010a候选物长期稳定性检验结果

Table 3. Long-term stability test results for GBW10010a candidate material

元素	X	RSD(%)	b₁	t_0.05×s(b₁)	U_s
Al	151.1	2.00	0.478	0.747	2.8
B	0.669	1.84	0.001	0.005	0.017
Ba	0.155	4.75	-0.001	0.002	0.008
Be	0.85	6.51	0.009	0.014	0.052
Bi	1.732	5.96	-0.012	0.032	0.12
Ca	68.54	1.29	0.038	0.328	1.2
Cd	54.04	1.44	0.026	0.293	1.1
Ce	5.203	5.18	-0.035	0.080	0.3
Co	6.544	3.70	0.025	0.080	0.3
Cr	0.085	6.23	0.000	0.002	0.008
Cs	3.687	2.71	0.005	0.037	0.14
Cu	3.024	0.45	0.002	0.003	0.013
Fe	4.277	0.82	-0.005	0.010	0.039
Ge	2.019	4.48	0.009	0.030	0.11
K	914.3	0.23	-0.239	0.668	2.5
La	2.94	5.50	-0.018	0.052	0.2
Li	16.78	7.92	-0.195	0.357	1.3
Mg	130.8	1.79	-0.424	0.437	1.6
Mn	10.89	2.18	-0.031	0.070	0.26
Mo	0.408	2.69	-0.001	0.004	0.015
Na	12.23	2.68	-0.056	0.071	0.27
Ni	0.205	0.92	0.000	0.001	0.003
P	838.6	0.25	-0.182	0.734	2.8
Pb	0.109	3.27	0.000	0.001	0.005
Rb	1.709	1.55	-0.003	0.008	0.031
S	1026	0.23	-0.009	0.881	3.3
Sb	10.62	1.75	-0.005	0.070	0.26
Sr	0.146	4.41	0.001	0.001	0.006
Y	218.6	2.49	-0.129	2.054	7.8
Yb	0.188	4.50	0.001	0.002	0.008
Zn	13.48	0.44	-0.006	0.019	0.071
Zr	7.104	0.41	-0.003	0.010	0.037
注：X均为2次测试的平均值；b₁为直线的斜率；t_0.05×s(b₁)为自由度95%的学生分布列表值；U_s为稳定性引入的不确定度分量。Bi、Cd、Ce、Co、Cs、Ge、La、Li、Y、Yb的质量分数为10^-9，其余元素的质量分数为10^-6。

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表 4 GBW10010a候选物短期稳定性检验结果

Table 4. Short-term stability test results for GBW10010a candidate material

元素	X	RSD(%)	b₁	t_0.05×s(b₁)
Al	151.1	1.41	0.182	1.141
B	0.667	2.00	0.000	0.008
Ba	0.153	4.38	-0.001	0.003
Bi	1.725	7.30	-0.018	0.050
Ca	68.5	2.63	0.127	0.995
Cd	54.0	1.87	0.112	0.494
Ce	5.27	5.65	-0.049	0.095
Co	6.61	2.92	0.019	0.099
Cr	0.086	6.98	0.000	0.004
Cs	3.68	2.94	-0.004	0.063
Cu	3.04	1.14	0.005	0.015
Fe	4.30	0.31	-0.001	0.007
Ge	2.05	4.18	0.010	0.040
K	916.3	1.28	0.251	6.942
La	2.95	6.34	-0.028	0.073
Li	16.4	7.91	-0.175	0.558
Mg	131.6	2.00	-0.347	1.157
Mn	10.8	2.59	-0.011	0.163
Mo	0.402	1.96	-0.001	0.004
Na	12.34	3.35	-0.061	0.160
Ni	0.202	1.95	0.001	0.001
P	839.0	1.19	-1.488	3.788
Pb	0.109	3.01	0.000	0.002
S	1011	1.53	-2.150	6.440
Sr	0.148	4.26	0.001	0.003
Y	215.8	1.35	-0.013	1.727
Yb	0.189	4.17	0.001	0.004
Zn	13.49	0.891	-0.017	0.050
注：X为2次测试的平均值; b₁为直线的斜率; t_0.05×s(b₁)为自由度95%的学生分布列表值。

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表 5 GBW10010a元素定值方法

Table 5. Sample decomposition methods and analytical methods for GBW10010a

元素	数据数	样品前处理方法	定值方法
Ag	7	DAC，DFMW	ICP-MS(7)
Al	7	DAC，FU	ICP-OES(6)，ICP-MS(1)
As	11	DAC，DAMW，DFMW，DMA	ICP-MS(6)，AFS(4)，ICP-OES(1)
B	11	DAC，DAMW，DFMW	ICP-MS(7)，ICP-OES(3)，ES(1)
Ba	11	DAC，DAMW，DFMW	ICP-MS(8)，ICP-OES(3)
Be	9	DAC，DAMW，DFMW	ICP-MS(9)
Bi	9	DAC，DFMW，DMA，DP	ICP-MS(8)，XRF(1)
Br	5	DAC，FU	ICP-MS(5)
Ca	10	DAC，DAMW，DFMW	ICP-OES(8)，ICP-MS(2)
Cd	11	DAC，DAMW，DFMW，DP	ICP-MS(10)，XRF(1)
Ce	10	DAC，DAMW	ICP-MS(10)
Cl	6	DAC，DP，FU	COL(4)，IC(1)，XRF(1)
Co	10	DAC，DAMW，DFMW	ICP-MS(10)
Cr	11	DAC，DAMW，DFMW	ICP-MS(11)
Cs	9	DAC，DAMW，DFMW	ICP-MS(9)
Cu	12	DAC，DAMW，DFMW	ICP-MS(10)，ICP-OES(2)
Dy	9	DAC，DAMW，DFMW	ICP-MS(9)
Er	9	DAC，DAMW，DFMW	ICP-MS(9)
Eu	9	DAC，DAMW，DFMW	ICP-MS(9)
F	5	DAC，DS，FU	ISE(2)，COL(2)，IC(1)
Fe	8	DAC，DAMW，DFMW	ICP-OES(6)，ICP-MS(2)
Gd	9	DAC，DAMW，DFMW	ICP-MS(9)
Ge	7	DAC，DAMW，DFMW	ICP-MS(7)
Hg	10	DAC，DAMW，DFMW，DMA	AFS(6)，ICP-MS(4)
Ho	10	DAC，DAMW，DFMW	ICP-MS(10)
I	5	DAC，DAMW，FU	ICP-MS(4)，COL(1)
K	10	DAC，DAMW，DFMW	ICP-OES(9)，ICP-MS(1)
La	9	DAC，DAMW，DFMW	ICP-MS(9)
Li	11	DAC，DAMW，DFMW	ICP-MS(11)
Lu	9	DAC，DAMW，DFMW	ICP-MS(9)
Mg	9	DAC，DAMW，DFMW	ICP-OES(8)，ICP-MS(1)
Mn	13	DAC，DAMW，DFMW	ICP-OES(7)，ICP-MS(6)
Mo	11	DAC，DAMW，DFMW	ICP-MS(11)
N	7	DA，DAC，DS	VOL(7)
Na	11	DAC，DAMW，DFMW	ICP-OES(9)，ICP-MS(2)
Nb	4	DAC，DAMW	ICP-MS(4)
Nd	7	DAC，DAMW	ICP-MS(7)
Ni	10	DAC，DAMW	ICP-MS(10)
P	10	DAC，DAMW，DFMW	ICP-OES(8)，ICP-MS(2)
Pb	10	DAC，DAMW，DFMW	ICP-MS(10)
Pr	9	DAC，DAMW，DFMW	ICP-MS(9)
Rb	11	DAC，DAMW，DFMW	ICP-MS(11)
S	10	DAC，DAMW，DFMW	ICP-OES(8)，ICP-MS(2)
Sb	8	DAC，DAMW，DFMW	ICP-MS(6)，AFS(2)
Sc	9	DAC，DAMW，DFMW	ICP-MS(9)
Se	9	DAC，DAMW，DMA	AFS(5)，ICP-MS(4)
Si	8	DAC，DP，FU	ICP-OES(7)，DP-XRF(1)
Sm	10	DAC，DAMW，DFMW	ICP-MS(10)
Sn	9	DAC，DAMW，DFMW	ICP-MS(8)，ES(1)
Sr	11	DAC，DAMW，DFMW	ICP-MS(7)，ICP-OES(4)
Tb	9	DAC，DAMW，DFMW	ICP-MS(9)
Th	8	DAC，DAMW，DFMW	ICP-MS(8)
Ti	9	DAC，DAMW，DFMW	ICP-MS(6)，ICP-OES(3)
Tl	7	DAC，DAMW，DFMW	ICP-MS(7)
Tm	9	DAC，DAMW，DFMW	ICP-MS(9)
U	9	DAC，DAMW，DFMW	ICP-MS(9)
V	8	DAC，DAMW，DFMW	ICP-MS(8)
Y	10	DAC，DAMW，DFMW	ICP-MS(10)
Yb	9	DAC，DAMW，DFMW	ICP-MS(9)
Zn	12	DAC，DAMW，DFMW	ICP-MS(9)，ICP-OES(3)
注：分解与富集方法：DAC—硝酸加过氧化氢密闭分解；DFMW—硝酸加氢氟酸微波消解；FU—碱熔或艾斯卡熔融；DAMW—硝酸加过氧化氢微波消解；DMA—混合酸分解；DP—粉末压片法；DS—硫酸分解。测定方法：ICP-MS—电感耦合等离子体质谱法；ICP-OES—电感耦合等离子体发射光谱法；AFS—原子荧光光谱法；XRF—X射线荧光光谱法；ES—直流电弧发射光谱法；COL—分光光度法；IC—离子色谱法；ISE—离子选择电极法；VOL—容量法。括号内的数字代表分析测试方法使用次数。

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表 6 GBW10010a认定值与不确定度

Table 6. Certified values and expanded uncertainty for GBW10010a

元素	认定值与不确定度(×10^-6)
Ag	0.004±0.001
Al^*	0.015±0.001
As	0.08±0.01
B	0.7±0.2
Ba	0.15±0.03
Be^**	-0.7
Bi^**	-1.4
Br	-
Ca^*	0.007±0.001
Cd^**	53±4
Ce	0.004±0.002
Cl^*	-
Co	0.006±0.002
Cr	-0.08
Cs	0.003±0.001
Cu	3.0±0.2
Dy^**	0.32±0.08
Er^**	0.19±0.05
Eu^**	-0.2
F	-
Fe	4.0±0.8
Gd^**	-0.3
Ge^**	-1.8
Hg^**	4.2±0.6
Ho^**	-0.1
I
K^*	0.090±0.005
La	(2.6)^**
Li	0.016±0.004
Lu^**	-0.04
Mg^*	0.013±0.001
Mn	11.1±0.7
Mo	0.42±0.04
N^*	1.30±0.05
Na	11.8±1.6
Nb	(1.3)^**
Nd	1.0±0.3^**
Ni	0.21±0.02
P^*	0.078±0.003
Pb	0.10±0.02
Pr^**	0.5±0.2
Rb	1.8±0.2
S^*	0.10±0.01
Sb	0.009±0.003
Sc^**	-6
Se	0.036±0.008
Si	48±15
Sm^**	0.3±0.1
Sn	-
Sr	0.15±0.03
Tb^**	0.07±0.03
Th^**	-1
Ti	-
Tl^**	0.23±0.05
Tm^**	-0.05
U^**	-0.8
V	-0.02
Y	0.21±0.05
Yb^**	0.19±0.05
Zn	13.3±1.2
注：带“”的元素含量单位为10^-2；带“*”的元素含量单位为10^-⁹；“-”为该元素未分析测试。

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表 7 GBW10010与GBW10010a定值数据对比

Table 7. Comparison of certified values between GBW10010 and GBW10010a

元素	定值(×10^-6)
元素	GBW10010	GBW10010a
Ag	-	0.004±0.001
Al^*	0.039±0.004	0.015±0.001
As	0.102±0.008	0.08±0.01
B	0.92±0.14	0.7±0.2
Ba	0.40±0.09	0.15±0.03
Be^**	1.8±0.4	(0.7)
Bi^**	(2.0)	(1.4)
Br	0.56±0.13	-
Ca^*	0.011±0.001	0.007±0.001
Cd^**	87±5	53±4
Ce	0.011±0.002	0.004±0.002
Cl^*	0.040±0.004	-
Co	(0.010)	0.006±0.002
Cr	(0.09)	(0.08)
Cs	0.014±0.005	0.003±0.001
Cu	4.9±0.3	3.0±0.2
Dy^**	(0.8)	0.32±0.08
Er^**	(0.32)	0.19±0.05
Eu^**	(0.3)	(0.2)
Fe	7.6±1.9	4.0±0.8
Gd^**	(0.75)	(0.3)
Ge^**	(5)	(1.8)
Hf	(0.12)	-
Hg^**	5.3±0.5	4.2±0.6
Ho^**	(0.12)	(0.1)
I	(0.09)	-
K^*	0.138±0.007	0.090±0.005
La	0.008±0.003	(0.0026)
Li	0.044±0.007	0.016±0.004
Lu^**	(0.04)	(0.04)
Mg^*	0.041±0.006	0.013±0.001
Mn	17±1	11.1±0.7
Mo	0.53±0.05	0.42±0.04
N^*	1.61±0.04	1.30±0.05
Na	25±8	11.8±1.6
Nb^**	-	(1.3)
Nd^**	(4)	1.0±0.3
Ni	0.27±0.02	0.21±0.02
P^*	0.136±0.006	0.078±0.003
Pb	0.08±0.03	0.10±0.02
Pr^**	1.1±0.3	0.5±0.2
Rb	3.9±0.3	1.8±0.2
S^*	0.147±0.024	0.10±0.01
Sb	(0.004)	0.009±0.003
Sc^**	(2.5)	(6)
Se	0.061±0.015	0.036±0.008
Si^*	0.025±0.003	0.048±0.015
Sm^**	(0.9)	0.3±0.1
Sr	0.30±0.05	0.15±0.03
Tb^**	(0.10)	0.07±0.03
Th^**	(4)	(1)
Ti	(2)	-
Tl^**	(0.7)	0.23±0.05
Tm^**	(0.05)	(0.05)
U^**	(1.2)	(0.8)
V	(0.03)	(0.02)
Y	0.052±0.009	0.21±0.05
Yb^**	(0.3)	0.19±0.05
Zn	23±2	13.3±1.2
灰分^*	(0.8)	-
注：带“”的元素质量分数为10^-2；带“*”的元素质量分数为10^-9；“±”后的数据为不确定度；括号内数据为参考值；“-”为该元素未分析测试。

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