GB/T 13883-2023 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 13883-2023 | English | 230 |
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Determination of selenium in feeds
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| GB/T 13883-2008 | English | 85 |
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Determination of selenium in feeds
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| GB/T 13883-1992 | English | 199 |
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Method for the determination of selenium in feedstuffs. (DAN) fluorometrt
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Excerpted PDFs (Download full copy in 9 seconds upon purchase)PDF Preview: GB/T 13883-2023
GB/T 13883-2023: Determination of selenium in feeds---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT13883-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.120
CCS B 46
Replacing GB/T 13883-2008
Determination of selenium in feeds
Issued on. AUGUST 06, 2023
Implemented on. MARCH 01, 2024
Issued by. State Administration for Market Regulation;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Terms and definitions... 4
4 Hydride generation-atomic fluorescence spectrometry (arbitration method)... 4
5 Fluorescence spectrophotometry... 9
6 Inductively coupled plasma mass spectrometry... 13
Annex A (informative) Reference conditions for microwave digestion... 18
1 Scope
This document describes the determination of selenium in feeds by hydride generation-
atomic fluorescence spectrometry, fluorescence spectrophotometry and inductively
coupled plasma-mass spectrometry.
In this document, hydride generation-atomic fluorescence spectrometry and
fluorescence spectrophotometry are applicable to the determination of selenium in
compound feed, concentrated feed, concentrate supplement, additive premix feed and
feed raw materials. Inductively coupled plasma mass spectrometry is applicable to the
determination of selenium in compound feed, concentrated feed, concentrate
supplement and feed raw materials (except mineral feed raw materials).
When the sample size is 1 g and the fixed volume is 50 mL, the detection limit of
hydride generation-atomic fluorescence spectrometry and fluorescence
spectrophotometry is 0.01 mg/kg and the quantification limit is 0.02 mg/kg. When the
sample size is 0.5 g and the fixed volume is 50 mL, the detection limit of inductively
coupled plasma mass spectrometry is 0.01 mg/kg and the quantification limit is 0.02
mg/kg.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 6682, Water for analytical laboratory use - Specification and test methods
GB/T 20195, Animal feed - Preparation of test samples
3 Terms and definitions
There are no terms or definitions that require definition in this document.
4 Hydride generation-atomic fluorescence spectrometry (arbitration method)
4.1 Principle
After the specimen is digested with acid, the selenium in the specimen digestion
solution is reduced to tetravalent selenium in the hydrochloric acid medium. Potassium
borohydride is used as a reducing agent to reduce tetravalent selenium to hydrogen
selenide in the hydrochloric acid medium.
4.2 Reagents or materials
Warning -- All strong acids shall be handled with caution. Dilution and use shall
be carried out in a fume hood. When using perchloric acid, be careful not to burn
it dry. Be careful of explosion.
4.2.17 Argon. the purity is not less than 99.995%.
4.3 Instruments and equipment
4.4 Sample
Prepare the specimen according to GB/T 20195, at least 200 g. Crush the compound
feed, concentrated feed, concentrate supplement and feed raw materials so that they all
pass through a 0.425 mm analysis sieve. Crush the additive premix feed so that they all
pass through a 0.25 mm analysis sieve. Mix well. Put into a sealed container and set
aside.
4.5 Test steps
4.5.1 Preparation of specimen solution
4.5.4 Determination
Adjust the instrument to the best working state. Start the measurement after stabilizing
for 15 min~20 min. Use hydrochloric acid solution II (4.2.10) as the carrier and
potassium borohydride solution (4.2.12) as the reducing agent. Use the carrier solution
for continuous injection.
4.6 Test data processing
The selenium content w1 in the specimen is expressed as mass fraction. The value is
expressed in milligrams per kilogram (mg/kg), calculated according to formula (1).
4.7 Precision
The ratio of the absolute difference between two independent determination results
obtained under repeatability conditions and their arithmetic mean to the arithmetic
mean shall meet the requirements of Table 1.
5 Fluorescence spectrophotometry
5.1 Principle
The specimen is digested with mixed acid, and selenium (Se4+) and 2,3-
diaminonaphthalene (DAN) generate 4,5-phenylbenzoselenadiazole in a slightly acidic
solution. The resulting complex is extracted with cyclohexane.
5.2 Reagents or materials
Warning -- All strong acids shall be handled with caution. Dilution and use shall
be carried out in a fume hood. When using perchloric acid, be careful not to burn
it dry. Be careful of explosion.
5.2.1 Water. GB/T 6682, Grade II.
5.2.2 Perchloric acid. guaranteed reagent.
Selenium content/(mg/kg) Relative deviation/%
5.2.3 Nitric acid. guaranteed reagent.
5.3 Instruments and equipment
5.4 Sample
Same as 4.4.
5.5 Test steps
5.5.1 Preparation of specimen solution
5.5.1.1 Wet digestion
5.5.2 Extraction
Add 2 drops of cresol red indicator (5.2.12) to the sample digestion solution. Adjust
with ammonia solution (5.2.7) until the solution turns yellow. Adjust with hydrochloric
acid solution III (5.2.8) until the solution turns orange (pH 1.5~2), then add 3 mL of
hydroxylamine hydrochloride-ethylenediaminetetraacetic acid disodium solution
(5.2.10). Shake well. Add 2 mL of 2,3-diaminonaphthalene solution (5.2.11).
5.6 Test data processing
The selenium content w2 in the specimen is expressed as mass fraction. The value is
expressed in milligrams per kilogram (mg/kg), calculated according to formula (2).
6 Inductively coupled plasma mass spectrometry
6.1 Principle
The specimen is digested with acid to dissolve selenium. Under certain acidic
conditions, it is introduced into an inductively coupled plasma mass spectrometer for
determination.
6.2 Reagents or materials
Selenium content/(mg/kg) Relative deviation/%
Warning -- All strong acids shall be handled with caution. Dilution and use shall
be done in a fume hood. When using perchloric acid, be careful not to burn it dry.
Be careful of explosion.
6.2.5 Hydrogen peroxide.
6.2.6 Nitric acid solution I. Take 5 mL of nitric acid (6.2.3) and add it to 95 mL of water.
Mix well.
6.2.7 Nitric acid solution II. Measure 30 mL of nitric acid (6.2.3) and add it to 70 mL
of water. Mix well.
6.4 Sample
Same as 4.4.
6.5 Test steps
6.5.1 Preparation of specimen solution
Perform two tests in parallel. Weigh 0.5 g of the specimen (accurate to 0.0001 g) into a
digestion tank. Add 8 mL of nitric acid (6.2.3). Soak for 10 min. Add 2 mL of hydrogen
peroxide (6.2.5).
6.5.2 Instrument reference conditions
The instrument reference conditions are as follows.
6.5.3 Determination
Adjust the instrument to the best working state. Calibrate with rhodium (103Rh) as
internal standard. Add rhodium internal standard element working solution (6.2.13)
online.
6.6 Test data processing
The selenium content w3 in the specimen is expressed as mass fraction, in milligrams
per kilogram (mg/kg), and is calculated according to formula (3).
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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