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標(biāo)題: 幫忙翻譯一個(gè)氟的檢測(cè)方法 [打印本頁(yè)]

作者: 叮當(dāng) 時(shí)間: 2009-4-22 16:10
標(biāo)題: 幫忙翻譯一個(gè)氟的檢測(cè)方法
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.

作者: bonderic 時(shí)間: 2009-4-25 20:27
看誰(shuí)想練下翻譯水平又有時(shí)間的幫一下忙。版主有獎(jiǎng)勵(lì)

作者: wxj1982 時(shí)間: 2009-4-26 10:22

氟的檢測(cè)

主題	氟
方法類(lèi)型	見(jiàn)第2頁(yè)
檢測(cè)范圍	動(dòng)物飼料和飼料原料 N.B.: 本方法不適于檢測(cè)礦物質(zhì)原料中氟的含量
最低檢測(cè)限	20 mg/kg
重復(fù)性	88 mg/kg at a level of 463 mg/kg (95% 可信區(qū)間 k=2)
重現(xiàn)性	141 mg/kg at a level of 463 mg/kg (95% reliability interval, k=2)
標(biāo)題	氟含量的檢測(cè) Labco WVS-022.DOC 第6版 2004.7

1. 定義

氟的含量的測(cè)定
2使用范圍

本方法適用于動(dòng)物飼料（原料）
3 原理

樣品經(jīng)鹽酸溶液提取、卡瑞試劑去除蛋白后，利用離子選擇電極檢測(cè)其氟的含量
4. 試劑要求
除特殊要求外，所有試劑均為分析純
R1 標(biāo)準(zhǔn)品

滴定液;濃度1000mg/L，定容1L 。
R2 1M 鹽酸溶液：
132.3ml鹽酸（R12），用水定容到10000ml
保質(zhì)期：室溫保存__ 年；
R3 3M 醋酸鈉溶液
溶解408g醋酸鈉(R13)于900 ml水中，用冰醋酸(R10) 調(diào)pH到7.00±0.10，定容到1000ml。
保質(zhì)期: 室溫保存3個(gè)月；
R4 檸檬酸鈉溶液：1.32M
溶解222g檸檬酸(R14)于250ml水中，加入28ml高氯酸(R7),定容至1000ml。
保質(zhì)期：室溫保存3個(gè)月；
R5 純化試劑I（據(jù)Carrez）

亞鐵氰化鉀(R11)265g，溶解并定容至2500ml。
保質(zhì)期：室溫保存3個(gè)月
R6純化試劑II（據(jù)Carrez）
乙酸鋅547.5g (R9)
97% 冰醋酸 75ml(R10)
用水溶解并定容至2500ml。
保質(zhì)期：室溫保存3個(gè)月

R7
0-72%高氯酸
R8 Tisab III (總離子強(qiáng)度校正緩沖溶液：
如：默克，產(chǎn)品號(hào)1.16770, 或相當(dāng)產(chǎn)品)
R9 二水合醋酸鋅
Zn(CH3COO)2.2H2O
R10 冰醋酸 97%, CH3COOH
R11 三水合亞鐵氰化鉀 K4[Fe(CN)6].3H2O
R12 鹽酸 24%
R13 三水合乙酸鈉
R14 二水合檸檬酸鈉
5. 設(shè)備和材料
T1 500 ml 塑料量瓶

T2攪拌器
T3 離子計(jì)：帶有
氟離子選擇電極
參比電極
T4 微量移液管, 1 ml 和5 ml
T5 pH 計(jì)

T6 塑料燒杯t, 100 ml ，帶攪拌桿
T7 移液管, 25 ml
T8 塑料燒杯, 600 ml
T9 塑料漏斗
T10 折疊濾紙：S&S 595 1/2
6. 樣品前處理

依據(jù)當(dāng)?shù)仄毡槭褂玫臉?biāo)準(zhǔn)處理程序
7. 方法
7.1 質(zhì)量控制
每組分析樣品必須帶有一個(gè)質(zhì)控樣品
7.2 稱量/提取
以下分析請(qǐng)?jiān)谕L(fēng)廚內(nèi)操作；
稱取一定量的樣品于500ml量瓶（T1）中，使氟的濃度在1000 μg（每500ml），加入50ml 1M鹽酸溶液，并攪拌60分鐘（R2, T2）；然后加入125ml醋酸鈉溶液(R3)和125ml檸檬酸鈉溶液(R4)，混合均勻；加入5ml 卡瑞試劑I并攪拌完全，再加入5ml 卡瑞試劑 II，再次攪拌完全，定容到刻度，混合均勻，過(guò)濾樣品(T8, T9, T10)。
移取25ml濾液到100ml燒杯中(T6, T7)，加入2.5ml Tisab試劑（R8）(pH = 5.4 + 0.2).
根據(jù)標(biāo)準(zhǔn)溶液加入法，利用帶有氟選擇電極的離子計(jì)，定量計(jì)算出氟的含量(T3, T4 和T5)。
8. 8 計(jì)算
c x V
F = ---------

g

式中：
F = 氟的含量，單位mg/kg;
c = 測(cè)試樣品中氟的濃度，單位μg/ml;
V = 樣品的稀釋倍數(shù)
g = 樣品質(zhì)量，單位g
9. 報(bào)告

結(jié)果報(bào)告如下：

當(dāng)含量低于檢測(cè)限時(shí)，F(xiàn) < 20mg/Kg

當(dāng)含量等于或高于檢測(cè)限時(shí)，F(xiàn)：***mg/Kg

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