Some standard content:
1 Scope
Chemical Industry Standard of the People's Republic of China
Feed grade
Ethoxyquin (ethoxyquinoline)
Feed grade Ethoxyquin
HG36942001
This standard specifies the requirements, test methods, inspection rules, marking, packaging, transportation, storage, etc. of feed grade ethoxyquin (ethoxyquinoline).
This standard applies to feed grade ethoxyquin made from p-nitrophenylacetaldehyde and acetone. This product is mainly used as an antioxidant in the feed industry.
Chemical name: 6-ethoxy-12-dihydro-2,2,4-trimethylquino-line
Molecular formula: CuH.NO
Structural formula:
Relative molecular mass: 217.31 (according to the 1999 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601—1988
GB/T6021988
GB/T603—1988
Chemical reagents-Preparation of standard solutions for titration analysis (volume analysis)Chemical reagents
Preparation of standard solutions for impurity determination (neqISO6353-1:1982)Preparation of preparations and products used in chemical reagent test methods (negISO6353-:1982)GB/T6678--1986
GB/T6682—1992
GB/T7531—1987
GB/T8450—1987
GB/T 8451—1987
General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987)Determination of ash content of organic chemical products
Determination method for ash in food additives
Test method for limit of heavy metals in food additives GB/T9725-1988
General rules for potentiometric titration of chemical reagents
GB106481999Feed labeling
Pharmacopoeia of the People's Republic of China 2000 edition Part II Appendix XA Solution color inspection method 3 Requirements
3.1 Properties: Yellow to brown viscous liquid, the color gradually darkens when placed in light and air, and the product tends to become a paste when stored at low temperature, with a slightly special smell.
Approved by the State Economic and Trade Commission on January 24, 2002, and implemented on July 1, 2002
HG3694—2001
3.2 The quality of feed-grade ethoxyquin should meet the requirements of Table 1. Table 1 Requirements
Ethoxyquin content (in C.HgNO), %Heavy metal content (in Pb), %
Monument content (in As), %
Ignition residue content, %Www.bzxZ.net
Solution properties
Note: Heavy metal content and arsenic content are mandatory indicators, and the rest are recommended indicators. 4 Test method
Compliance with regulations
The reagents used in this test method are analytical pure reagents, and the water used is the third-grade water specified in GB/T6682. The standard solutions, impurity standard solutions, preparations and products used in this test method shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified. 4.1 Identification test
The sample is prepared into a 1:10000 n-hexane solution and irradiated under ultraviolet light with a wavelength of 365nm to emit a dark white fluorescence. The sample is prepared into a 1:20000 isopropanol solution and measured by spectrophotometry. The maximum absorption is at a wavelength of 356-362nm.
4.2 Determination of ethoxyazole content
4.2.1 Potentiometric method (arbitration method)
4.2.1.1 Summary of the method
Under non-aqueous conditions, the sample is titrated with a standard perchloric acid titration solution to carry out a neutralization reaction, and the potentiometer indicates the end point. 4.2.1.2 Instruments
a) Acidity meter or potentiometer: with an accuracy of 0.1 pH unit or 10 mV. b) Electrode: Glass-saturated calomel electrode. 4.2.1.3 Reagents and solutions
a) Glacial acetic acid.
b) Acetic anhydride.
e) Perfluoric acid standard titration solution: c(HCIO,)=0.1 mol/L. 4.2.1.4 Analysis steps
Install the instrument and electrode according to the requirements of GB/T9725. Weigh 0.2g of the sample (accurate to 0.0002g), put it in a dry beaker, add 50mL of glacial acetic acid and 1mL of acetic anhydride, insert the electrode into the beaker and immerse it in the solution, start the stirrer, and titrate with perchloric acid standard titration solution until the maximum potential jump no longer recovers as the end point. Perform a blank test at the same time.
4.2.1.5 Expression of analysis results
The content of ethoxyquin (in terms of CuHrNO) expressed as mass percentage (X,) is calculated according to formula (1): Xi = c(V-Vo)X0. 217 3×100
-actual concentration of perchloric acid standard titration solution, mol/L, where: c
-actual volume of perchloric acid standard titration solution consumed by the sample, mLV. Volume of perchloric acid standard titration solution consumed by the blank test, mL; 20
-mass of the sample in g;
HG3694—2001
-mass of ethoxyquin expressed in grams equivalent to 1.00mL perchloric acid standard titration solution [c(HCIO,)=1.000mol/L].
The arithmetic mean of the results of two parallel determinations is taken as the determination result. The difference between the results of two parallel determinations shall not exceed 0.3%. 4.2.2 Indicator method
4.2.2.1 Method summary
Under non-aqueous conditions, titrate the sample with a perchloric acid standard titration solution to carry out a neutralization reaction, and the indicator indicates the end point. 4.2.2.2 Reagents and solutions
a) Glacial acetic acid.
b) Acetic anhydride.
e) Perchloric acid standard titration solution: c(HCIO.)=0.1mol/L. d) Methyl violet indicator: 10g/L glacial acetic acid solution. Weigh 1g of methyl violet, dissolve it with an appropriate amount of glacial acetic acid, transfer it to a 100mL volumetric flask, and dilute it to the scale with glacial acetic acid. 4.2.2.3 Analysis steps
Weigh about 0.2g of the sample (accurate to 0.0002g), add 50mL of glacial acetic acid and 1mL of acetic anhydride into a dry and clean conical flask, add 2 drops of methyl violet indicator, and titrate with pernitrogen acid standard titration solution until it turns blue-green. Perform a blank test at the same time.
4.2.2.4 Expression of analysis results
Perform in accordance with 4.2.1.5.
4.3 Determination of heavy metal content
Perform in accordance with GB/T8451. Among them: Lead standard solution: 0.01mgPb per milliliter of solution. Take 10.0mL of solution containing 0.1mgPb per milliliter in a 100mL volumetric flask and dilute to the mark. Prepare before use. Weigh 5g of the sample (accurate to 0.002g), and the sample treatment is carried out according to the dry digestion method. During the determination, take 10mL of sample solution and accurately measure 1.0mL of lead standard solution.
4.4 Determination of arsenic content
Perform according to the provisions of GB/T8450 arsenic spot method. Among them: Standard solution: 0.001mgAs per milliliter of solution. Take 1mL of solution containing 0.1mgAs per milliliter in a 100mL volumetric flask and dilute to the scale.
Weigh 5g of sample (accurate to 0.0002g), and the sample treatment is carried out according to the method of digestion. During the determination, take 10mL of sample solution and accurately measure 2.0mL of arsenic standard solution.
4.5 Determination of ignition residue content
4.5.1 Analysis steps
Weigh 5g of sample (accurate to 0.0002g), and perform according to the provisions of GB/T7531. Ignition temperature (650±25)℃. 4.5.2 Expression of analysis results
The ignition residue content (X2) expressed as a percentage by mass is calculated according to formula (2): Xz=m=ma×100
The mass of the sample, g;
Where: m
The mass of a crucible plus the residue, m;
-The mass of the crucible, g.
Take the arithmetic mean of the results of two parallel determinations as the determination result. The difference between the results of two parallel determinations shall not exceed 0.02%. 4.6 Properties of the solution
HG3694—2001
4.6.1 Reagents and solutions
4.6.1.1 Nitride cobalt solution for colorimetry: Prepare according to the method specified in Appendix XA Solution Color Test Method of Part II of the Pharmacopoeia of the People's Republic of China 2000 Edition.
4.6.1.2 Copper sulfate solution for colorimetry: Prepare according to the method specified in Appendix Zone A Solution Color Test Method of Part II of the Pharmacopoeia of the People's Republic of China 2000 Edition.
4.6.1.3 Potassium dichromate solution for colorimetry: Prepare according to the method specified in Appendix XA Solution Color Test Method of Part II of the Pharmacopoeia of the People's Republic of China 2000 Edition.
4.6.1.4 Mixed colorimetric solution: Mix 7.5mL of chlorinated cobalt solution for colorimetry, 5mL of copper sulfate solution for colorimetry and 7.5mL of potassium dichromate solution for colorimetry.
4.6.2 Analysis steps
Weigh 1.0g of the sample and add 20mL of n-hexane. The solution should be clear. The color of the solution should not be darker than the mixed colorimetric solution. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2. The quality inspection department of the manufacturer shall inspect the quality of feed-grade ethoxyquin batch by batch according to the provisions of this standard. The manufacturer shall ensure that the products shipped meet the requirements of this standard. 5.3 The maximum amount of ethoxyquin in each batch shall not exceed 20t. 5.4 The number of sampling units shall be determined in accordance with the provisions of 6.6 of GB/T6678-1986. The total amount of sampling shall not be less than 500mL. Use a glass tube with a diameter of 13mm and a length of 1m with a thinner end to collect samples. The samples collected should include the upper, middle and lower parts of the barrel. Mix the selected samples and divide them into two clean and dry brown glass bottles with ground stoppers and affix labels with the manufacturer name, product name, batch number, production date, sampling date and the name of the sampler. One bottle is for inspection and the other bottle is kept for reference. 5.5 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling and re-inspection shall be carried out from twice the number of packaging units. If there is still one index that does not meet the requirements of this standard in the re-inspection results, the batch of products shall be judged as unqualified. 6 Marking, packaging, transportation and storage
6.1 Ethoxyazole should be packaged in clean and dry 25kg polyethylene plastic barrels or 200kg iron barrels, or packaged according to the user's requirements. 6.2 The packaging should have firm and clear markings, including the product name, manufacturer's name, factory address, production license number, product approval number, this standard number, and trademark. Product labels should comply with the provisions of GB10648. 6.3 During transportation and storage, loading and unloading should be handled gently, and vehicles and ships should be clean. It is strictly forbidden to mix and store with toxic and harmful substances or other contaminated items. When storing, it should be sealed and placed in a cool place to avoid direct sunlight. 6.4 Under the conditions specified in this standard, the shelf life is 10 months from the date of production. Products that have exceeded the shelf life can continue to be used if they meet the requirements of this standard after inspection.
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