GB/T 13079-2022 PDF English
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GB/T 13079-2022 | English | 215 |
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Determination of total arsenic in feeds
| Valid |
GB/T 13079-2006 | English | 230 |
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Determination of total arsenic in feeds
| Obsolete |
GB/T 13079-1999 | English | 359 |
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Determination of total arsenic in feeds
| Obsolete |
GB/T 13079-1991 | English | RFQ |
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Method for determination of total arsenic in feeds
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GB/T 13079-2022: Determination of total arsenic 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/GBT13079-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.120
CCS B 46
Replacing GB/T 13079-2006
Determination of Total Arsenic in Feeds
Issued on. DECEMBER 30, 2022
Implemented on. JULY 1, 2023
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative References... 5
3 Terms and Definitions... 5
4 Silver Salt Method (arbitration method)... 5
5 Hydride Generation-atomic Fluorescence Spectrometry... 12
6 Inductively Coupled Plasma Mass Spectrometry... 18
Appendix A (informative) Microwave Digestion Reference Conditions... 23
1 Scope
This document describes the silver salt method, hydride generation-atomic fluorescence
spectrometry and inductively coupled plasma mass spectrometry for the determination of total
arsenic in feeds.
This document is applicable to the determination of total arsenic in compound feeds,
concentrated feeds, concentrate supplements, additive premixed feeds, feedstuffs and feed
additives.
When the sampling size is 5 g and the constant volume is 50 mL, the detection limit of the silver
salt method is 0.25 mg/kg and the quantitation limit is 0.50 mg/kg; when the sampling size is 5
g, the constant volume is 50 mL and the dilution factor is 20, the detection limit of the hydride
generation-atomic fluorescence spectrometry and inductively coupled plasma mass
spectrometry is 0.02 mg/kg, and the quantitation limit is 0.05 mg/kg.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in the text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
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
This document does not have terms or definitions that need to be defined.
4 Silver Salt Method (arbitration method)
4.1 Principle
After a specimen is treated by acid digestion, direct acid dissolution or dry ashing method, use
potassium iodide and stannous chloride to reduce high-valent arsenic to trivalent arsenic, then,
generate arsine with the new ecological hydrogen produced by zinc particles and acid, which is
absorbed by the silver diethyldithiocarbamate (Ag-DDTC)-triethylamine-chloroform solution
to form a red jelly, whose color shade is proportional to the arsenic content.
4.2 Reagents or Materials
WARNING---handle all kinds of strong acids with caution. Dilute and use them in a fume
hood. When using perchloric acid, be careful not to burn it to dryness, and be careful of
explosion.
4.3 Instruments and Equipment
4.3.1 Spectrophotometer. with a wavelength accuracy of 2 nm.
4.3.2 Analytical balance. with an accuracy of 0.0001 g.
4.3.3 Electric drying oven. with a temperature control accuracy of 5 C.
4.4 Sample
In accordance with GB/T 20195, prepare the sample of at least 200 g. Make it all pass through
the analysis sieve with a pore size of 0.425 mm, thoroughly mix it, put it into a closed container
and set it aside.
4.5.2 Determination
4.5.2.1 Preparation of standard series of solutions
Accurately transfer-take 0.00 mL, 1.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL and 10.00
mL of the arsenic standard intermediate solution (4.2.20), respectively place them in arsenic
reaction bottle, and use water to dilute to 30 mL. Add 10 mL of hydrochloric acid (4.2.3), mix
it well, and follow the steps specified in 4.5.2.2, starting from the addition of 2 mL of potassium
iodide solution (4.2.12).
4.6 Test Data Processing
The total arsenic content w1 in the specimen, which is expressed in mass fraction and (mg/kg),
is calculated in accordance with Formula (1).
4.7 Precision
The ratio of the absolute difference between the two independent determination results obtained
under repeatability conditions and their arithmetic mean, and the arithmetic mean shall comply
with the requirements of Table 1.
5 Hydride Generation-atomic Fluorescence Spectrometry
5.1 Principle
After a specimen is treated by acid digestion, direct acid dissolution or dry ashing method, add
thiourea to pre-reduce pentavalent arsenic to trivalent arsenic, then, in an acidic environment,
reduce it with potassium borohydride to generate gaseous arsine, which is loaded into a quartz
atomizer by argon gas and decomposed into atomic arsenic. Under the excitation of the emitted
light of an arsenic hollow cathode lamp, generate atomic fluorescence, whose fluorescence
intensity is proportional to the concentration of arsenic in the determined solution. Adopt the
external standard method for quantitative determination.
5.2 Reagents or Materials
WARNING---handle all kinds of strong acids with caution. Dilute and use them in a fume
hood. When using perchloric acid, be careful not to burn it to dryness, and be careful of
explosion.
Unless otherwise specified, use only analytically pure reagents.
5.2.1 Water. GB/T 6682, Grade-1.
5.2.2 Nitric acid. guaranteed reagent.
5.2.3 Hydrochloric acid. guaranteed reagent.
5.2.4 Sulfuric acid. guaranteed reagent.
5.2.5 Hydrogen peroxide.
5.2.6 Magnesium oxide.
Total Arsenic Content (w1)/(mg/kg) Relative Deviation/%
5.2.7 Magnesium nitrate.
5.2.8 Potassium hydroxide. guaranteed reagent.
5.2.9 Potassium borohydride. guaranteed reagent.
5.3 Instruments and Equipment
5.3.1 Atomic fluorescence spectrophotometer.
5.3.2 Analytical balance. with an accuracy of 0.0001 g.
5.4 Sample
Same as 4.4.
5.5 Test Procedures
5.5.4 Instrument reference conditions
The instrument reference conditions are as follows.
5.5.5 Determination
Adjust the atomic fluorescence spectrophotometer to the optimum working condition,
successively determine the fluorescence intensity value of the standard series of solutions, blank
solution and specimen solution. Take the concentration of the standard series of solutions as the
x-coordinate and the fluorescence intensity value as the y-coordinate to draw a standard curve,
with a correlation coefficient of r 0.995.When the fluorescence value of the specimen solution
exceeds the linear range of the curve, reduce the dispensing volume of the specimen solution,
in accordance with 5.5.3 and 5.5.4, re-perform the determination. In order to ensure good
repeatability of the determination results, it is recommended that the number of sequences for
each determination should not exceed 30 (including the number of curve sequences).
5.6 Test Data Processing
The total arsenic content w2 in the specimen, which is expressed in mass fraction and (mg/kg),
is calculated in accordance with Formula (2).
6 Inductively Coupled Plasma Mass Spectrometry
6.1 Principle
After a specimen is treated by acid digestion, direct acid dissolution or dry ashing method,
dilute it into a specimen test solution, which is atomized and sent into the ICP torch by the
carrier gas. Through evaporation, dissociation, atomization and ionization, convert it into
charged ions, which enter the mass spectrometer through the ion collection system.
6.2 Reagents or Materials
WARNING---handle all kinds of strong acids with caution. Dilute and use them in a fume
hood. When using perchloric acid, be careful not to burn it to dryness, and be careful of
explosion.
6.2.1 Water. GB/T 6682, Grade-1.
6.2.2 Nitric acid. guaranteed reagent.
6.2.3 Hydrochloric acid. guaranteed reagent.
6.2.4 Sulfuric acid. guaranteed reagent.
6.2.5 Hydrogen peroxide.
6.2.6 Magnesium oxide.
6.2.7 Magnesium nitrate.
Total Arsenic Content (w2)/(mg/kg) Relative Deviation/%
6.3 Instruments and Equipment
6.3.1 Inductively coupled plasma mass spectrometer.
6.3.2 Analytical balance. with an accuracy of 0.0001 g.
6.3.5 Adjustable electric furnace.
6.3.6 Graphite digestion instrument. equipped with matching polytetrafluoroethylene digestion
tube.
6.3.7 Microwave digestion instrument. equipped with matching polytetrafluoroethylene
digestion tube.
6.3.8 High-pressure digestion tank. equipped with matching polytetrafluoroethylene digestion
inner tube.
6.5.3 Instrument reference conditions and interference elimination method
6.5.3.1 Instrument reference conditions
The instrument reference conditions are as follows.
6.5.4 Determination
Adjust the instrument to the optimum working condition, add the internal standard working
solution (6.2.17) online, use 5% nitric acid solution for zero-adjustment, and successively
determine the signal intensity of arsenic (75As) in the standard series of solutions (6.2.18), blank
test solution (6.5.2) and specimen test solution (6.5.2). Take the concentration of the standard
series of solutions as the x-coordinate and the signal intensity as the y-coordinate to draw a
standard curve, with a correlation coefficient of the standard curve r 0.999.When the response
value of the specimen solution exceeds the linear range of the curve, the acid concentration of
the standard series of solutions can be appropriately diluted and determined, so as to ensure that
the response value of the specimen solution is within the linear range of the curve.
6.6 Test Data Processing
The total arsenic content w3 in the specimen, which is expressed in mass fraction and (mg/kg),
is calculated in accordance with 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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