Standard Reference Material of Orchard Leaves
果树叶标样
1 Scope of Application
This leaf sample (red star apple) is in possession of the standard reference value of the contents of such mineral elements as nitrogen, phosphorus, potassium, calcium, magnesium, ferrum, copper, manganese, zinc and boron, which may be used to verified the accuracy of the analysis result for the above-mentioned ten elements, as well as used in calibration instrument and for the inspection or establishment of new methods.
2 Preparation
In the middle of June, 1982, 30,000 pieces of red star apple leaves had been sampled from the Chang Yang orchard in the suburb of Beijing. After the process of washing, drying and pulverizing as well as being sieved and mixed repeatedly for three times, an uniform sample of 4 kg had been obtained and then been sub-packaged in 12 1000mL polyethylene plastic bottles.
The leaf sample was dried for 12h in a 85℃ drying oven within the plastic bottle and radiated with Cobalt-60 gamma-ray 4.9 Mrad by Atomic Energy Research Institute of Chinese Academy of Agricultural Sciences after sealing the cap; then it was sealed up and stored in dark places under room temperature (10 ~ 30℃).
3 Fineness and Uniformity
3.1 Fineness: more than 98 % of the particles shall pass through 60-mesh and 50 % of the particles shall pass through 160-mesh.
3.2 Uniformity: take 3 sub-samples from each of the 12 plastic bottles storing the leaf samples in order to repeat for 3 times; carry out the determination of nitrogen and phosphorus contents and check the obtained data with F; if there is no significant difference in the result, then the sample is proved to be uniform.
4 Standard Reference Value for the Standard Reference Material of Orchard Leaves
The analyzing and value setting shall be carried out through such ten analysis techniques as Kjeldahl method, Dumas method, atomic absorption method, neutron activation analysis method, inductively coupled plasma atomic emission spectrometry and the like by domestic and foreign laboratories with certain analytic level; several laboratories shall take similar standard substance of the U.S. as reference.
The value setting for each element shall be carried out with more than two analysis methods which are of different principles and there shall be provided with analysis data from more than six laboratories. After being treated with statistic methods, the average value, 95% confidence limit and coefficient of variation are listed in the following table.
Standard Reference Value for the Standard Reference Material of Orchard Leaves
Element data number n Average value of content 95% confidence limit Coefficient of variation, %
Invariable element (%dry basis*)
N
P
K
Ca
Mg 13
9
14
14
12 2.42
0.176
1.61
1.48
0.471 2.36~2.48
0.166~0.186
1.51~1.71
1.42~1.54
0.433~0.509 3.9
8.1
10.8
6.7
11.5
Trace element (mg/kg dry basis*)
Fe
Cu
Mn
Zn
B 11
10
10
11
7 117
31.8
25.2
14.8
36.1 108~126
29.5~34.1
24.6~25.8
14.1~15.5
32.8~39.4 12.0
10.0
3.5
6.7
10.2
*Counted by dry basis dried for 4h at 85℃. .
5 Packaging, Preservation and Application Method of Standard Reference Material
This standard reference material is packaged within plastic bottles with 20g in each bottle; the bottle neck is equipped with plastic inner cover and the outer cover is sealed with plastic cement.
5.1 This standard reference material shall be preserved in dark and dry places with the temperature not exceeding 30℃.
5.2 Prior to use, the standard reference material shall be mixed uniformly again and dried for 4 h in a 85℃ drying oven; then it shall be placed in a dryer and weighed after cooling.
5.3 The amount of standard reference material for general analysis shall not be less than 0.5g.
6 Supply Organization
Mineral Nutrition Research Center of College of Horticulture, China Agricultural University.
1 Scope of Application
2 Preparation
3 Fineness and Uniformity
4 Standard Reference Value for the Standard Reference Material of Orchard Leaves
5 Packaging, Preservation and Application Method of Standard Reference Material
6 Supply Organization
Appendix A Analytical Method and Determination Organization of Standard Leaf Sample of Orchards (Supplement)
中华人民共和国国家标准
果树叶标样
Standard reference material of orchard leaves
UDC 631.1/.8：581.45(086.0)
GB 7171-87
1 适用范围
本叶样(红星苹果)具有矿质元素氮、磷、钾、钙、镁、铁、铜、锰、锌、硼含量的标准参比值，可用于鉴定对上述十种元素分析结果的准确程度，校准仪器，检验或建立新的方法。
2 制备
1982年6月中旬，在北京郊区长阳果园，采取了3万片红星苹果叶片，经过洗涤、烘干、粉碎后，反复三次过筛混合，得到均一的样本4 kg，分装于12个1000ml聚乙烯塑料瓶中。
叶样在塑料瓶内于85℃烘箱干燥12h，封盖后由中国农科院原子能研究所经钴-60γ射线4.9Mrad照射后，在室温下(10～30℃)封存于暗处。
3细度、均匀度
3.1 细度；98‰以上的颗粒通过60目，50％的颗粒通过160目。
3.2 均匀度：从贮放叶样的12个塑料瓶的每瓶内，各取3个分样作为3次重复，进行氮、磷含量测定，所得数据用F检验，结果无显著差异，证明样品是均匀的。
4果树叶标样的标准参比值
分析定值由国内外具有一定分析水平的实验室，使用开氏法、杜马法、原子吸收法、中子活化分析法、电感耦合等离子体发射光谱法等10种分析技术测定，部分实验室用美国同类标准物质作参比。
每种元素的定值均用两种以上不同原理的分析方法。有六个实验室以上的分析数据。经统计方法处理，其平均值、95%置信限和变异系数列于下表。
果树叶样标准参比值
元素数据数n 含量平均值 95％置信限 变异系数，％
常置元素(％干基*)
N
P
K
Ca
Mg 13
9
14
14
12 2.42
0.176
1.61
1.48
0.471 2.36～2.48
0.166～0.186
1.51～1.71
1.42～1.54
0.433～0.500 3.9
8.1
10.8
6.7
11.5
*以85℃干燥4 h干基计。
续表
元素数据数n 含量平均值 95％置信限 变异系数，%
微量元素(mg，kg/干基*)
Fe
Cu
Mn
Zn
B 11
10
10
11
7 117
31.8
25.2
14.8
36.1 108～126
29.5～34.1
24.6～25.8
14.1～15.5
32.8～39.4 12.0
10.0
3.5
6.7
10.2
*以85℃干燥4 h干基计。
5标样的包装、保存和使用方法
本标样包装在塑料瓶中，每瓶20g，瓶口加塑料内盖，外盖加塑胶密封。
5.1 避光、干燥保存，温度不超过30℃。
5.2 使用前应再度混匀，在85℃温度烘箱内烘4 h，置干煤器内，冷却后称重。
5.3 一般分析方法用样量不少于0.5g。
6 供应单位
北京农业大学园艺系果树矿质营养研究室。
附录A
果树标准叶样的分析方法和测定单位
(补充件)
分析方法*
测定单位**
元素 A B C D E F G H I J
N 1,3,4,5,6,7,10.12,15,16 14 9
P 15,16 1,3,4,B,10,12,14 9
K 4,6 2,10,11,14 15,16 9,8
Ca 2,3,4,6,11,14 14 15,16 8,9 10
Mg 2,3,4,6,11,14 15,16 9 10
Fe 2,3,4,6,11,14 15,16 8,9 10
Cu 2,3,4,6,11,14 15,16 9
Mn 2,3,4,6,11,14 15,16
9
Zn 2,3,4,6,11,14 15,16 8,9
B 14,15 1,3,12
*分析方法；
A 凯氏法或改良凯氏法；
B 杜马法；
C 原子吸收分光光度法；
D 火焰光度法；
E 电感耦合等离子体发射光谱法；
F 钒钼黄(或磷钼蓝)比色法；
G 甲亚胺比色法；
H 中子活化法；
I EDTA容量法；
J 邻菲啰啉比色法。
**测定单位：
1 北京农业大学园艺乐果树矿质营养研究室；
2 北京农业大学土化系无机分板教研组；
3 中国农科院综合分析室；
4 中国农科院土壤肥料所测试中心；
5 中国农科院郑州果树所土肥室；
6 中国农科院柑桔研究所；
7 中国农科院畜牧研究所；
9 北京师范大学低能核物理研究所；
9 广东省测试分析研究所；
10 山东省果树研究所化验室；
11 浙江科学院柑桔研究所；
12 新疆农科院中心试验室；
13 波兰科学院；
14 德意志联邦共和国霍因海姆大学植物营养研究所；
15 美国宾夕法尼亚大学植物分析实验室；
16 美国农部贝尔茨维尔研究中心果树研究室。
附加说明：
本标准由中华人民共和国农牧渔业部提出。
本标准由北京农业大学园艺系果树矿质营养研究室负责起草。
本标准主要起草人李港丽、苏润宇、沈隽。
