Standard Reference Material of Orchard Leaves
果樹葉標樣
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)
中華人民共和國國家標準
果樹葉標樣
Standard reference material of orchard leaves
UDC 631.1/.8：581.45(086.0)
GB 7171-87
1 適用范圍
本葉樣(紅星蘋果)具有礦質元素氮、磷、鉀、鈣、鎂、鐵、銅、錳、鋅、硼含量的標準參比值，可用于鑒定對上述十種元素分析結果的準確程度，校準儀器，檢驗或建立新的方法。
2 制備
1982年6月中旬，在北京郊區長陽果園，采取了3萬片紅星蘋果葉片，經過洗滌、烘干、粉碎后，反復三次過篩混合，得到均一的樣本4 kg，分裝于12個1000ml聚乙烯塑料瓶中。
葉樣在塑料瓶內于85℃烘箱干燥12h，封蓋后由中國農科院原子能研究所經鈷-60γ射線4.9Mrad照射后，在室溫下(10～30℃)封存于暗處。
3細度、均勻度
3.1 細度；98‰以上的顆粒通過60目，50％的顆粒通過160目。
3.2 均勻度：從貯放葉樣的12個塑料瓶的每瓶內，各取3個分樣作為3次重復，進行氮、磷含量測定，所得數據用F檢驗，結果無顯著差異，證明樣品是均勻的。
4果樹葉標樣的標準參比值
分析定值由國內外具有一定分析水平的實驗室，使用開氏法、杜馬法、原子吸收法、中子活化分析法、電感耦合等離子體發射光譜法等10種分析技術測定，部分實驗室用美國同類標準物質作參比。
每種元素的定值均用兩種以上不同原理的分析方法。有六個實驗室以上的分析數據。經統計方法處理，其平均值、95%置信限和變異系數列于下表。
果樹葉樣標準參比值
元素數據數n 含量平均值 95％置信限 變異系數，％
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干基計。
續表
元素數據數n 含量平均值 95％置信限 變異系數，%
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干基計。
5標樣的包裝、保存和使用方法
本標樣包裝在塑料瓶中，每瓶20g，瓶口加塑料內蓋，外蓋加塑膠密封。
5.1 避光、干燥保存，溫度不超過30℃。
5.2 使用前應再度混勻，在85℃溫度烘箱內烘4 h，置干煤器內，冷卻后稱重。
5.3 一般分析方法用樣量不少于0.5g。
6 供應單位
北京農業大學園藝系果樹礦質營養研究室。
附錄A
果樹標準葉樣的分析方法和測定單位
(補充件)
分析方法*
測定單位**
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 凱氏法或改良凱氏法；
B 杜馬法；
C 原子吸收分光光度法；
D 火焰光度法；
E 電感耦合等離子體發射光譜法；
F 釩鉬黃(或磷鉬藍)比色法；
G 甲亞胺比色法；
H 中子活化法；
I EDTA容量法；
J 鄰菲啰啉比色法。
**測定單位：
1 北京農業大學園藝樂果樹礦質營養研究室；
2 北京農業大學土化系無機分板教研組；
3 中國農科院綜合分析室；
4 中國農科院土壤肥料所測試中心；
5 中國農科院鄭州果樹所土肥室；
6 中國農科院柑桔研究所；
7 中國農科院畜牧研究所；
9 北京師范大學低能核物理研究所；
9 廣東省測試分析研究所；
10 山東省果樹研究所化驗室；
11 浙江科學院柑桔研究所；
12 新疆農科院中心試驗室；
13 波蘭科學院；
14 德意志聯邦共和國霍因海姆大學植物營養研究所；
15 美國賓夕法尼亞大學植物分析實驗室；
16 美國農部貝爾茨維爾研究中心果樹研究室。
附加說明：
本標準由中華人民共和國農牧漁業部提出。
本標準由北京農業大學園藝系果樹礦質營養研究室負責起草。
本標準主要起草人李港麗、蘇潤宇、沈雋。
