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GB 32449-2015: Feed additive -- Magnesium sulphate
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Feed additive -- Magnesium sulphate
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GB 32449-2015
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Basic data | Standard ID | GB 32449-2015 (GB32449-2015) | | Description (Translated English) | Feed additive -- Magnesium sulphate | | Sector / Industry | National Standard | | Classification of Chinese Standard | B46 | | Classification of International Standard | 65.120 | | Word Count Estimation | 9,980 | | Date of Issue | 2015-12-31 | | Date of Implementation | 2016-07-01 | | Regulation (derived from) | State Standard Announcement 2015 No.43 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | GB 32449-2015: Feed additive -- Magnesium sulphate---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Feed additive - Magnesium sulphate
ICS 65.120
B46
National Standards of People's Republic of China
Feed additive over magnesium
Published 2015-12-31
2016-07-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China issued
Foreword
This standard of Chapter 1, Chapter 3 and Chapter 5 are mandatory, the rest are recommended.
This standard was drafted in accordance with rules GB/T 1.1-2009 given.
This standard is proposed and managed by the National Feed Industry Standardization Technical Committee (SAC/TC76).
This standard was drafted. Beijing Institute of Animal Chinese Academy of Agricultural Sciences, Institute of Guangdong Academy of Agricultural Sciences, southerly chemical
Group Co., Ltd.
The main drafters. Lu Lin, Luo Xu Gang, BUSINESS STUDIES He Qixia, Zhang Liyang, Zhang Ling Yan, Ma Yunlong, Chen Aibing, Lv Hongxia.
Feed additive over magnesium
1 Scope
This standard specifies requirements for a feed additive or over anhydrous magnesium sulfate heptahydrate, test methods, inspection rules, labeling, packaging, transportation,
Storage and shelf life.
This standard applies to the chemical synthesis method or a sulfuric acid salt lake bittern production of a feed additive or over anhydrous magnesium sulfate heptahydrate.
Molecular formula. MgSO4 · nH2O, n = 1 or n = 7.
Molecular Weight. 138.38 (n = 1), 246.47 (n = 7) (according to 2007 international relative atomic mass).
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
General Method GB/T 3051-2000 inorganic chemical products chloride content measured by the mercury Method
GB T6003.1-2012 Test sieves of metal wire cloth
GB/T 6682 Water for analytical laboratory specifications and test methods
GB 10648 feed tag
Determination GB/T 13079-2006 total arsenic in feed
GB/T 13080-2004 lead in Feed Atomic Absorption Spectrometry
Determination GB/T 13081 feed Mercury
GB/T 14699.1 feed samples
Preparation GB/T 601 standard titration solution Chemicals
3.1 Appearance and traits
A product as a white anhydrous magnesium sulfate (sulfate chemical synthesis) or off-white powder (Salt Lake bittern method), magnesium sulphate heptahydrate as a colorless crystalline particles
Particles without agglomeration.
3.2 Technical Specifications
Feed additives over magnesium to comply with Table 1.
Table 1 Specifications
project
index
An anhydrous magnesium
MgSO4 · H2O
Magnesium sulfate heptahydrate
MgSO4 · 7H2O
Magnesium sulfate (MgSO4) /% ≥94.0 ≥99.0
Magnesium (Mg) /% ≥16.5 > 9.7
TABLE 1 (cont.)
project
index
An anhydrous magnesium
MgSO4 · H2O
Magnesium sulfate heptahydrate
MgSO4 · 7H2O
Total arsenic (As)/(mg/kg) ≤2
Lead (Pb)/(mg/kg) ≤2
Mercury (Hg)/(mg/kg) ≤0.2
Chloride (Cl) /%
Sulfate Chemical synthesis. ≤0.1
Salt Lake Bittern method. ≤1.5
Sulfate Chemical synthesis. ≤0.1
Salt Lake Bittern method. ≤1.0
Clarity test Clarification
Fineness (400μm test sieve) /% ≥95 -
Test Method 4
Warning. some of the procedures specified test methods can lead to dangerous situations, the operator should take appropriate safety and health practices.
The standard test methods the reagents and water, in the absence of other requirements specified, are by analytical reagent 6682 and GB/T in
Three water.
4.1 sensory testing
The appropriate amount of sample is placed in a clean white paper, color and observed under natural light state.
4.2 Identification Test
4.2.1 Reagents and materials
4.2.1.1 solution of ammonium chloride. 50g/L.
4.2.1.2 ammonia solution. aqueous ammonia = 23.
4.2.1.3 ammonium carbonate solution (200g/L). Weigh 20g of ammonium carbonate, aqueous ammonia 20mL was added, water was added to 100mL.
4.2.1.4 sodium dihydrogen phosphate solution (50g/L). Weigh 5g of sodium dihydrogen phosphate, add appropriate amount of water dissolved, add water to 100mL.
4.2.1.5 barium chloride solution (50g/L). Weigh 5g barium chloride, add appropriate amount of water dissolved, add water to 100mL.
4.2.2 Analysis of step
Identification of magnesium ions 4.2.2.1
The sample was dissolved in water, was added aqueous ammonia solution (4.2.1.2), i.e., a white precipitate of ammonium chloride was added dropwise a solution of (4.2.1.1), the precipitate was dissolved again
Was added a solution of sodium dihydrogen phosphate (4.2.1.4) to form a white precipitate, this precipitate was not dissolved in the ammonia.
Identification of sulfate ion 4.2.2.2
The sample was dissolved in water, a solution of barium chloride (4.2.1.5), a white precipitate formed.
4.3 Determination of magnesium sulfate and magnesium content
4.3.1 Principle
Masking with a small amount of triethanolamine of trivalent iron and aluminum ions added pH≈10 ammonia - ammonium chloride buffer solution, chrome black T as indicator.
The total amount of disodium ethylenediaminetetraacetate (EDTA) titration standard titration solution calcium and magnesium.
Under the conditions of the test solution pH≈12.5 to the Cal as indicator, with disodium ethylenediaminetetraacetic acid (EDTA) Standard
Titration titration of calcium. Subtracting from the total amount of calcium and magnesium in the calcium content, to calculate the magnesium content.
4.3.2 Reagents
4.3.2.1 ammonia solution. aqueous ammonia = 12.
4.3.2.2 triethanolamine. Triethanolamine water = 13.
4.3.2.3 ammonia - ammonium chloride buffer solution (pH≈10). Weigh 27g of ammonium chloride, dissolved in appropriate amount of water, add 197 mL of aqueous ammonia, diluted with water to
500mL.
4.3.2.4 sodium hydroxide solution. 50g/L.
4.3.2.5 disodium edetate (EDTA) standard titration solution [c (EDTA) = 0.05mol/L]. prepared according to GB/T 601 requirements.
4.3.2.6 disodium edetate (EDTA) standard titration solution [c (EDTA) = 0.02mol/L]. prepared according to GB/T 601 requirements.
4.3.2.7 chrome black T indicator. 5g/L.
4.3.2.8 indicator in the Cal. Cal - 0.1g taken and dried for 2h at 105 ℃ NaCl10g, milled
Mix well.
4.3.3 Analysis of step
4.3.3.1 Preparation of test solution
Weigh about 10g of magnesium sulfate heptahydrate or a 5g sample over anhydrous magnesium sulfate, accurate to 0.0001g, was placed in a 250mL beaker was added 100mL
Dissolved in water. All transferred to 250mL volumetric flask, diluted with water to the mark. If necessary dry filtration, the solution was a solution A, for
Determination of calcium and magnesium content, calcium content, the chloride content.
4.3.3.2 Determination
Determination of calcium and magnesium content 4.3.3.2.1
Pipette with a pipette 10mL solution A, placed in 250mL Erlenmeyer flask, was added 40mL of water, 5 mL triethanolamine (4.3.2.2), with
Aqueous ammonia solution (4.3.2.1) adjusted to pH 7-8, was added 10mL of ammonia - ammonium chloride buffer solution (4.3.2.3) and a small amount of Eriochrome Black T (4.3.2.7),
With disodium edetate Standard Solution (4.3.2.5) to the solution titrated from purple to pure blue as the end point.
At the same time a blank test. Pipette with a pipette 10mL of water, placed in 250mL Erlenmeyer flask, and the kind of operation and other reagents were added
Are the same number of assays.
4.3.3.2.2 Determination of calcium content
Pipette with a pipette 10mL solution A, placed in 250mL Erlenmeyer flask, was added 25mL of water, 5 mL of triethanolamine solution (4.3.2.2).
5mL sodium hydroxide solution was added with shaking (4.3.2.4), plus a small amount in the Cal indicator (4.3.2.8), labeled with disodium edetate
Quasi titration solution (4.3.2.6) to the solution titrated from purple to pure blue as the end point.
At the same time a blank test. Pipette with a pipette 10mL of water, placed in 250mL Erlenmeyer flask, other types of operations and the addition of reagents
And number are the same assay.
4.3.4 Calculation of results showing
X1 to a magnesium content of over anhydrous magnesium sulfate (MgSO4 · H2O) [or magnesium sulfate heptahydrate (MgSO4 · 7H2O), or magnesium (of Mg)]
The mass fraction, expressed in% value, calculated according to formula (1).
X1 =
25 × (V1-V1,0) c1M1 × 10-3
m × 100-λX2 =
2.5 × (V1-V1,0) c1M1
m -λX2
(1)
X2 calcium content of calcium (Ca) mass fraction, expressed in%, calculated according to formula (2).
X2 =
25 × (V2-V2,0) c2M2 × 10-3
m × 100 =
2.5 × (V2-V2,0) c2M2
(2)
Where.
C1 --- disodium ethylenediaminetetraacetate (EDTA) accurate value of the concentration of the standard titration solution (4.3.2.5) in units of moles per liter
(Mol/L);
Volume (EDTA) Standard Solution (4.3.2.5) the titration of the sample Vl --- calcium and magnesium total number of consumed Disodium ethylenediaminetetraacetate
Value in milliliters (mL);
Blank Test Titration of Calcium and Magnesium in the total amount of consumed V1,0 --- disodium edetate (EDTA) Standard Solution (4.3.2.5) of the body
Product of value, in milliliters (mL);
C2 --- disodium ethylenediaminetetraacetate (EDTA) accurate value of the concentration of the standard titration solution (4.3.2.6) in units of moles per liter
(Mol/L);
V2 --- titration sample content of calcium disodium edetate consumption (EDTA) standard titration solution volume value (4.3.2.6), and
Milliliters (mL);
V2,0 --- blank titration calcium content consumed disodium edetate (EDTA) titration volume of standard solution (4.3.2.6) of
Value in milliliters (mL);
--- m sample mass value in grams (G);
--- magnesium sulfate with a Ml product over anhydrous magnesium sulfate (MgSO4 · H2O) timing, the value of its molar mass M (MgSO4 · H2O) =
138.4 [or magnesium sulfate heptahydrate (MgSO4 · 7H2O) timing, the value of its molar mass M (MgSO4 · 7H2O) =
246.5; or magnesium (Mg) timing, the value of its molar mass M (Mg) = 24.31], in units of grams per mole (g/mol);
--- M2 numerical molar mass of calcium (Ca), in units of grams per mole (g/mol) (M2 = 40.08);
[lambda] --- magnesium sulfate to a product over anhydrous magnesium sulfate (MgSO4 · H2O) timing, scaling factor [lambda] Calcium (MgSO4 · H2O) = 3.453
[Or magnesium sulfate heptahydrate (MgSO4 · 7H2O) timing, λ (MgSO4 · 7H2O) = 6.150; or magnesium (Mg) timing,
λ (Mg) = 0.6065].
In the arithmetic mean of the two determination results parallel the measurement results, the result to one decimal place reserved.
The absolute difference determination results MgSO4 · 7H2O parallel to no more than 0.5%, to no more than MgSO4 · H2O
0.3%, to no more than 0.05% Mg.
4.4 Determination of Arsenic
According to GB/T 13079-2006 measurement Chapter 5, wherein the sample processing carried out in 5.4.1.2.1.
4.5 Determination of lead content
According to GB/T 13080-2004 assay in which the sample is dissolved in GB/T 13080-2004 performed in 7.1.2.1. Measurement sample required buckle
In addition to background.
4.6 Determination of mercury content
Measured by GB/T 13081.
4.7 Determination of chloride (Cl) content
4.7.1 Principle
With GB/T 3051-2000 Chapter 3.
4.7.2 Reagents
4.7.2.1 mercuric nitrate standard titration solution. c [1/2Hg (NO3) 2] = 0.05mol/L, according to GB/T 3051-2000 with a predetermined 4.6
And system calibration.
4.7.2.2 The remaining 3051-2000 Chapter 4 with GB/T .
4.7.3 instruments and equipment
With GB/T 3051-2000 Chapter 5.
4.7.4 Analysis of step
Pipette with a pipette 50mL solution A (4.3.3.1), placed in 250mL Erlenmeyer flask, add 3 drops of bromophenol blue indicator solution was added dropwise nitric acid
Solution just turns from blue to yellow, and then an excess of 5 drops. Add 1mL diphenylcarbazone hydrazide indicator solution, using microburette, with nitric acid
Mercury standard solution was titrated to titrate the solution from yellow to purple, is the end.
At the same time a blank test. Pipette with a pipette 50mL of water, placed in 250mL Erlenmeyer flask, other types of operations and the addition of reagents
And number are the same assay.
The waste liquid after titration saved, processing predetermined GB/T 3051-2000 of Appendix D.
4.7.5 Calculation of results showing
X3 chloride content of chlorine (Cl) mass fraction, expressed in%, calculated according to formula (3).
X3 =
5 × (V3-V3,0) c3M3 × 10-3
m × 100 =
0.5 × (V3-V3,0) c3M3
(3)
Where.
Numerical volume V3 --- mercury nitrate titration standard solution (4.7.2.1) titration test solution consumed, in milliliters (mL);
Values V3,0 --- volume of mercury nitrate titration standard solution (4.7.2.1) titration of the blank test solution consumed, in units of ml
(ML);
C3 --- accurate value of the concentration of mercury nitrate Standard Solution (4.7.2.1), in units of moles per liter (mol/L);
--- M3 molar mass of chlorine (Cl) values, in units of grams per mole (g/mol) (M = 35.45);
--- m sample mass values, in units of grams (g).
In the arithmetic mean of the two determination results parallel the measurement results, the result to one decimal place reserved.
The absolute difference between the two measurement results in terms of magnesium sulfate heptahydrate not more than 0.01% to not greater than a water 0.1% magnesium.
4.8 Clarity test
Weigh 5.0g ± 0.1g sample was dissolved was added 20mL of water, the solution should be clear and transparent without white turbidity.
4.9 Determination of fineness
4.9.1 Principle
The test sample is sieved, particle size is determined by the mass of products in accordance with the sample test sieve.
4.9.2 instruments and equipment
Test sieve. φ200 × 50-0.4/0.25 GB/T 6003.1-2012.
4.9.3 Analysis of step
Weigh 10g sample accurately to 0.1g, placed in a test sieve, and the sieve cover fitted sieved undersize. In the horizontal direction two times/s.
Shaking speed, until no test sieve until the sample by collecting the undersize falls under the sieve, sieve mass was weighed to the nearest 0.1g.
4.9.4 Calculation of results showing
X4 fineness mass fraction, expressed in%, calculated according to formula (4).
X4 =
m1
m2
× 100 (4)
Where.
--- the mass M1 test sieve material in grams (G);
--- M2 sample mass, in grams (g).
The arithmetic average of the measurement results of two parallel measurement results, the results of a number of reservations to.
The absolute difference determination results parallel to less than 1%.
5 Inspection Rules
5.1 Batch
In the same material, the same production process, continuous production or shift production of the same products as a group, but each batch of products shall not exceed 60t.
5.2 Sampling
Predetermined sampling GB/T 14699.1's.
5.3 factory inspection
Sulfuric acid produced by chemical synthesis products test items. magnesium, total arsenic, lead. Salt Lake bittern production process product testing project. magnesium, total
Arsenic, lead, chloride.
5.4 Type inspection
Type test items for the full requirements of Chapter 3. When the product of normal production, at least once every six months type test, but with the following situation
When one condition, also type inspection.
A) The product type;
b) production processes or sources of raw materials has major changes, which may affect the product mass;
c) discontinued more than three months, to resume production;
D) When the factory test results and the last type test results are quite different.
5.5 determine the rules
When there is an indicator of the test results do not meet the requirements of this standard, should be re-double the amount of self-packaging sampling retest, retest results even
When there is an indicator does not meet the requirements of this standard, the entire batch of product is substandard.
6 labels, packaging, transport and storage
6.1 Label
Executed according to GB 10648, and indicate the name of the production process.
6.2 Packaging
Packaging materials should be non-toxic, harmless and moisture.
6.3 Transport
Transport packaging to prevent breakage, sun, rain, and toxic and hazardous substances prohibited Commonwealth Games.
6.4 Storage
Prevent storage sun, rain, toxic or harmful substances is prohibited reservoir.
7 Shelf Life
Under the provisions of the transportation, storage conditions, shelf life of 12 months.
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