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GB/T 13083-2018 (GBT 13083-2018)

GB/T 13083-2018_English: PDF (GBT13083-2018)
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BASIC DATA
Standard ID GB/T 13083-2018 (GB/T13083-2018)
Description (Translated English) Determination of fluorine in feeds -- Ion selective electrode method
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard B46
Classification of International Standard 65.120
Word Count Estimation 5,591
Date of Issue 2018-05-14
Date of Implementation 2018-12-01
Older Standard (superseded by this standard) GB/T 13083-2002
Drafting Organization Zhejiang Veterinary Drug Feeding Institute
Administrative Organization National Feed Industry Standardization Technical Committee (SAC/TC 76)
Regulation (derived from) National Standards Announcement No. 6 of 2018
Proposing organization National Feed Industry Standardization Technical Committee (SAC/TC 76)
Issuing agency(ies) State Administration of Markets and China National Standardization Administration

GB/T 13083-2018
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.120
B 46
Replacing GB/T 13083-2002
Determination of Fluorine in Feeds -
Ion Selective Electrode Method
ISSUED ON. MAY 14, 2018
IMPLEMENTED ON. DECEMBER 01, 2018
Issued by. State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Principle ... 4
4 Reagents and Materials ... 5
5 Apparatus ... 6
6 Sample Preparation ... 6
7 Test Procedures ... 6
8 Test Data Processing ... 8
9 Precision ... 8
Foreword
This Standard was drafted as per the rules specified in GB/T 1.1-2009.
This Standard replaced GB/T 13083-2002 Determination of Fluorine in Feed – Ion
Selective Electrode Method; compared with GB/T 13083-2002, this Standard has the
major technical changes as follows besides the editorial modifications.
--- Expand the scope of the standard “this Standard is applicable to feed, feed
ingredients, phosphate and mixed feed additive with aluminosilicate as carrier”;
--- Modify the detection limit of the method;
--- Modify the description of the principle;
--- Modify the measurement range of acidity meter and fluoride ion selective
electrode;
--- Increase the preparation method of stone powder sample of feed ingredients;
--- Increase the preparation method of mixed feed additive sample with
aluminosilicate as carrier;
--- The result shall be expressed from 0.1mg/kg to 1mg/kg.
This Standard was proposed by and under the jurisdiction of National Technical
Committee for Standardization of Feed Industry (SAC/TC 76).
Drafting organization of this Standard. Zhejiang Province Institute of Veterinary Drug
and Feedstuff.
Chief drafting staffs of this Standard. Ren Yuqin, Huang Juan, Zhang Zhijian, Zhu
Congying, Yuan Lu, Zhang Xiaoli, Qiu Chengjun, and Shang Xiaojin.
The historical editions replaced by this Standard are as follows.
--- GB/T 13083-1991, GB/T 13083-2002.
Determination of Fluorine in Feeds -
Ion Selective Electrode Method
1 Scope
This Standard specifies using ion selective electrode method to determine the fluorine
in the feeds.
This Standard is applicable to the feed, feed ingredients, phosphate and mixed feed
additive with aluminosilicate as carrier.
The detection limit of this method is 3mg/kg (take 1g of sample, make constant volume
to 50mL).
2 Normative References
The following documents are essential to the application of this document. For the
dated documents, only the versions with the dates indicated are applicable to this
document; for the undated documents, only the latest version (including all the
amendments) are applicable to this document.
GB/T 6682 Water for Analytical Laboratory Use – Specification and Test Methods
GB/T 14699.1 Feeding Stuffs – Sampling
GB/T 20195 Animal Feeding Stuffs – Preparation of Test Samples
3 Principle
The sample is extracted by hydrochloric acid solution; use total ionic strength buffer
solution to adjust the pH to be 5~6; eliminate the acidity and the ion interference such
as Al3+, Fe3+, Ca2+, Mg2+, and SiO32- that can form complexes with fluoride ion; then use
ion meter to measure the potential difference between the fluoride ion selective
electrode and the saturated calomel electrode; such potential difference is linear with
the logarithm of the fluoride ion activity (concentration) in the solution; use the linear
equation obtained by the potential difference measured by the fluorine standard series
with known concentration to find the fluoride ion concentration corresponding to the
potential difference of the unknown sample solution; calculate the fluorine content in
the sample.
5 Apparatus
5.1 Analytical balance. sensitivity of 0.0001g.
5.2 Ion meter. measuring range of 0.0mV~±1800mV; or its equivalent pH meter or
potentiometer.
5.3 Fluoride ion electrode. measuring range of 10-1 mol/L ~ 10-6 mol/L; pF-1 type or its
equivalent composite electrode.
5.4 Reference electrode. saturated calomel electrode or its equivalent electrode.
5.5 Electrothermal constant-temperature drying oven.
5.6 High temperature furnace.
5.7 Magnetic stirrer.
5.8 Ultrasonic extractor.
5.9 Nickel crucible or platinum crucible.
6 Sample Preparation
Take representative sample according to the provisions of GB/T 14699.1; take about
250g of reduced sample by quadruple method; prepare the sample as per the provision
of GB/T 20195; pulverize and pass through the analytical sieve with pore size of
0.425mm; mix evenly; place into the grinding bottle for later-use.
7 Test Procedures
7.1 Preparation of fluorine standard series
Accurately pipette 0.5mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL of fluorine standard
working solution II [4.7c)] and 2.00mL, 5.00mL of fluorine standard working solution I
[4.7b)]; separately place them into 50mL volumetric flasks; separately add 5.0mL of
hydrochloric acid solution (4.5), 25mL of total ionic strength buffer solution (4.4); add
water to the scale; mix evenly. The concentrations of the above standard series are
0.1µg/mL, 0.2µg/mL, 0.4µg/mL, 1.0µg/mL, 2.0µg/mL, 4.0µg/mL, 10.0µg/mL.
7.2 Preparation of sample solution
7.2.1 Preparation of feeds and feed ingredients (except for the three types listed
in 7.2.2, 7.2.3 and 7.2.4) sample solutions