帮忙翻译一个氟的检测方法

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11 F (Fluorine)

Substance	Fluorine
Type of method	see page 2
For investigation in	Animal feeds and animal feed raw materials N.B.: This method is not suitable for determining fluorine in mineral raw materials
Minimum determination limit	20 mg/kg
Repeatability	88 mg/kg at a level of 463 mg/kg (95% reliability interval, k=2)
Reproducibility	141 mg/kg at a level of 463 mg/kg (95% reliability interval, k=2)
Title	Determination of the fluorine content. Labco WVS-022.DOC version 6 July 2004

1. Definition
Determination of the fluorine content.
2. Intended area of use
The method is applicable to animal feed (raw materials).
3. Principle
The fluorine content is established with the assistance of an ion-selective electrode, after extraction with hydrochloric acid and deproteinisation with Carrez.
4. Reagents and requirements
All reagents and solvents must be of analysis quality, unless stated otherwise.
R1 Standard:
Titrisol fluoride: after topping up to 1 litre 1000 mg/l
R2 1M Hydrochloric acid:
132.3 ml hydrochloric acid (R12)
Demiwater up to 10000 ml
Shelf-life: _ years at room temperature
R3 3M Sodium acetate:
Dissolve 408 g sodium acetate (R13) in  900 ml of water.
Set the pH to 7.00  0.10 with acetic acid (R10) and top up to 1000 ml.
Shelf-life: 3 months at room temperature.
R4 Sodium citrate 1.32 M:
Dissolve 222 g sodium citrate (R14) in  250 ml of water.
Add 28 ml perchloric acid (R7) and top up to 1000 ml.
Shelf-life: 3 months at room temperature.
R5 Purification solution I (according to Carrez):
Potassium hexacyanoferrate II 265 g (R11)
Demiwater up to 2500 ml
Shelf-life: 3 months at room temperature.
R6 Purification solution II (according to Carrez):
Zinc acetate 547.5 g (R9)
Acetic acid 97% 75 ml (R10)
Demiwater up to 2500 ml
Shelf-life: 3 months at room temperature.
R7 Perchloric acid 70-72%
R8 Tisab III (total ionic strength adjustment buffer solution; e.g. Merck art. 1.16770, or equivalent)
R9 Zinc acetate dihydrate Zn(CH3COO)2.2H2O
R10 Glacial acetic acid 97%, CH3COOH
R11 Potassium hexacyanoferrate trihydrate K4[Fe(CN)6].3H2O
R12 Hydrochloric acid 24%
R13 Sodium acetate trihydrate
R14 Sodium citrate dihydrate
5. Equipment and resources
T1 500 ml plastic measuring flask
T2 Mixer/agitator
T3 Orion ion meter with:
- an ion-selective electrode for fluorine
- reference electrode
T4 Micropipettes, 1 ml and 5 ml
T5 pH meter
T6 Plastic beaker, 100 ml with stir bar
T7 Pipette, 25 ml
T8 Plastic beaker, 600 ml
T9 Plastic funnel
T10 Folded filter S&S 595 1/2
6. Sample pre-treatment
According to locally prevailing standard procedures
7. Method
7.1 Quality control
A control sample is taken for each series.
7.2 Weighing/extraction
Perform the analysis in duplo.
Weigh a quantity of sample material into a measuring flask (T1) of 500 ml in agreement with + 1000 μg fluorine (per 500 ml).
Add 50 ml hydrochloric acid 1M and stir for 60 minutes (R2, T2). Add 125 ml sodium acetate solution (R3) and 125 ml sodium citrate solution (R4) and mix. Add 5 ml Carrez I (R5) and agitate well. Then add 5 ml Carrez II (R6) and agitate well again. Top up to the line, mix and filter the sample (T8, T9, T10).
Pipette 25 ml into a 100 ml beaker (T6, T7) and add 2.5 ml Tisab (R8) (pH = 5.4 + 0.2).
Ascertain the concentration of fluorine by means of the standard addition method (R1) using an ion meter fitted with a fluoride electrode (T3, T4 and T5).
8. Calculation

c x V
F = ---------

g
where
F = Fluorine content, in mg/kg;
c = Concentration of fluorine present in the measured quantity sample, in μg/ml;
V = Conversion factor for the used dilution and quantity of the sample used for processing;
g = Weighed sample, in g.
9. Reporting
The outcome is reported as follows:
For a content less than the determinable limit:
Fluorine: less than 20 mg/kg
For a content equal to or greater than the determinable limit:
Fluorine: xxxx mg/kg
10. Characteristics
Demonstrable limit:
10 mg/kg
Determinable limit:
20 mg/kg
Repeatability:
88 mg/kg at a level of 463 mg/kg (95% reliability interval, k=2)
Reproducibility (in the laboratory):
141 mg/kg at a level of 463 mg/kg (95% reliability interval, k=2)
11. Quality control
The slope of the measurement must lie between 60 and 65.
12. Literature
AOAC Official Methods of Analyses 975.08. 15th edition 1990.
Fluorine in Animal Feed.

bonderic

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氟的检测

主题	氟
方法类型	见第2页
检测范围	动物饲料和饲料原料 N.B.: 本方法不适于检测矿物质原料中氟的含量
最低检测限	20 mg/kg
重复性	88 mg/kg at a level of 463 mg/kg (95% 可信区间 k=2)
重现性	141 mg/kg at a level of 463 mg/kg (95% reliability interval, k=2)
标题	氟含量的检测 Labco WVS-022.DOC 第6版 2004.7

1. 定义

氟的含量的测定
2使用范围

本方法适用于动物饲料（原料）
3 原理

  样品经盐酸溶液提取、卡瑞试剂去除蛋白后，利用离子选择电极检测其氟的含量
4. 试剂要求
除特殊要求外，所有试剂均为分析纯
R1 标准品

   滴定液;浓度1000mg/L，定容1L 。
R2 1M 盐酸溶液：
132.3ml盐酸（R12），用水定容到10000ml
保质期：室温保存__ 年；
R3 3M 醋酸钠溶液
溶解408g醋酸钠(R13)于900 ml水中，用冰醋酸(R10) 调pH到7.00±0.10，定容到1000ml。
保质期: 室温保存3个月；
R4 柠檬酸钠溶液：1.32M
溶解222g柠檬酸(R14)于250ml水中，加入28ml高氯酸(R7),定容至1000ml。
保质期：室温保存3个月；
R5 纯化试剂I（据Carrez）

亚铁氰化钾(R11)265g，溶解并定容至2500ml。
保质期：室温保存3个月
R6纯化试剂II（据Carrez）
乙酸锌547.5g (R9)
97% 冰醋酸 75ml(R10)
用水溶解并定容至2500ml。
保质期：室温保存3个月

R7
0-72%高氯酸
R8 Tisab III (总离子强度校正缓冲溶液：
如：默克，产品号1.16770, 或相当产品)
R9 二水合醋酸锌
Zn(CH3COO)2.2H2O
R10 冰醋酸 97%, CH3COOH
R11 三水合亚铁氰化钾 K4[Fe(CN)6].3H2O
R12 盐酸 24%
R13 三水合乙酸钠
R14 二水合柠檬酸钠
5. 设备和材料
T1 500 ml 塑料量瓶

T2搅拌器
T3 离子计：带有
氟离子选择电极
参比电极
T4 微量移液管, 1 ml 和5 ml
T5 pH 计

T6 塑料烧杯t, 100 ml ，带搅拌杆
T7 移液管, 25 ml
T8 塑料烧杯, 600 ml
T9 塑料漏斗
T10 折叠滤纸：S&S 595 1/2
6. 样品前处理


依据当地普遍使用的标准处理程序
7. 方法
7.1 质量控制
每组分析样品必须带有一个质控样品
7.2 称量/提取
以下分析请在通风厨内操作；
称取一定量的样品于500ml量瓶（T1）中，使氟的浓度在1000 μg（每500ml），加入50ml 1M盐酸溶液，并搅拌60分钟（R2, T2）；然后加入125ml醋酸钠溶液(R3)和125ml柠檬酸钠溶液(R4)，混合均匀；加入5ml 卡瑞试剂I并搅拌完全，再加入5ml 卡瑞试剂 II，再次搅拌完全，定容到刻度，混合均匀，过滤样品(T8, T9, T10)。
移取25ml滤液到100ml烧杯中(T6, T7)，加入2.5ml Tisab试剂（R8）(pH = 5.4 + 0.2).
根据标准溶液加入法，利用带有氟选择电极的离子计，定量计算出氟的含量(T3, T4 和T5)。
8.  8 计算
c x V
F = ---------

g

式中：
F = 氟的含量，单位mg/kg;
c = 测试样品中氟的浓度，单位μg/ml;
V = 样品的稀释倍数
g = 样品质量，单位g
9. 报告


结果报告如下：

当含量低于检测限时，F < 20mg/Kg

当含量等于或高于检测限时，F：***mg/Kg

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