Some standard content:
Record number: 3723--1999
HG 2941---1999
This standard is equivalent to the Japanese Feed Additive Safety Law Compendium (1995 Edition) "Choline Chloride" (hereinafter referred to as "Compendium") to revise the chemical industry standard HG2941-1989 "Feed Additive Choline Chloride". The main technical differences between this standard and the "Compendium" are: the content of choline fluoride in this standard is expressed in four specifications: 70%, 75% aqueous solution and 50%, 60% powder to meet the requirements of domestic production and trade; the content of choline chloride in the "Compendium" is expressed in two specifications: 70% aqueous solution and 90% to 110% (calculated as choline chloride) powder Specifications are indicated.
This standard does not have a drying loss item for aqueous solutions, but adds two items, drying loss and fineness, for powders. The ethylene glycol index is better than that in the "Essentials"; the others are the same as those in the "Essentials".
The sampling methods, signs, reagents, and writing formats in this standard are in compliance with relevant regulations in my country. The main technical differences between this standard and HG2941--1989 are: the chloroethanol process route has been cancelled in the scope; the chloroethanol item has been cancelled in the requirements. The specifications of 75% aqueous solution and 60% powder have been added. The technical requirements of these two specifications are the same as those of 70% aqueous solution and 50% powder; the fineness index of the powder has been changed from the original The previous 95% is changed to 90%. This standard is divided into two parts, including four specifications of products: 75%, 70% aqueous solution and 60%, 50% powder. Appendix A of this standard is the appendix of the standard.
This standard will replace HG2941-1989 from the date of implementation. This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the basic organic product standardization technical unit of the Ministry of Chemical Industry. The main drafting units of this standard: Shandong Chemical Research Institute, Shenyang Petrochemical Research Institute. Participating drafting units of this standard: Jinan Hualing Pharmaceutical Co., Ltd., Shanghai Spik Eubi Bile Chloride Co., Ltd., Tianjin Bohai Animal Drug Factory, Siping Lianhua Tianhua Industrial Corporation, Tianjin Animal Drug Erguang, Shaanxi Weinan Feed Additive Factory, Cangzhou Northern Animal Drug Factory. The main drafters of this standard are Zhang Guiqin, Shi Qi, and Lv Ruimin. This standard was first issued as a national standard in 1989, and was adjusted to a mandatory chemical industry standard in 1997 and renumbered. This standard is entrusted to the basic organic product standardization technical unit of the Ministry of Chemical Industry for interpretation. 185
1 Scope
Chemical Industry Standard of the People's Republic of China
Feed Grade
Choline Chloride
Feed grade-
Choline chloride
HG 2941--. 1999
Replaces HG2941---1989
This standard specifies the requirements, test methods, inspection rules, labeling, packaging, transportation, storage, etc. for feed grade choline fluoride aqueous solution (including 70% and 75%) and powders (including 50% and 60%) made from choline chloride aqueous solution with corn cob powder, defatted rice bran, rice husk powder, bran, anhydrous silicic acid and other excipients suitable for feed. This standard applies to choline chloride aqueous solution and its powder products produced by the reaction of trimethylamine hydrochloride aqueous solution and ethylene oxide. The structural formula of the main ingredient Choline chloride:
[HOCH,CH2—N+_CH,]CI
Molecular formula: C,HNCIO
Relative molecular mass: 139.63 (according to the 1995 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 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T602--1988 Preparation of standard solutions for determination of impurities in chemical reagents (negISO6353-1:1982) GB/T603-1988 Preparation of preparations and products used in test methods for chemical reagents (neqISO6353-1:1982) GB/T6003--1985 Test sieves
GB/T 6435---1986
GB/T 6678--1986
GB/T 6682-1992
CB/T 7531--1987
Determination method of moisture content in feed
General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories (negISO3696:1987) Determination of ash content in organic chemical products
GB10648—1993
Feed label
3 Common matters
Unless otherwise specified, the reagents used in this standard are analytically pure reagents. Water should meet the third-grade water specifications in GB/T6682. The standard titration solution, impurity standard solution, preparation and product used in this standard shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified. National Petroleum and Chemical Industry Fan 1999-06~16 Approved 186
2000-06-01 Implementation
4 Requirements
4.1 Properties
HG 2941—1999
Part I 70 %, 75% choline fluoride aqueous solution
4.1.1 This product is a colorless, transparent, viscous liquid with a slightly peculiar odor. 4.1.2 This product is miscible with water, methanol, and ethanol, but is almost insoluble in ether, chloroform, or benzene. 4.1.3 This product is hygroscopic and releases an amine odor when it absorbs carbon dioxide. 4.2 70% and 75% choline chloride aqueous solutions shall meet the requirements of Table 1. Table 1 Requirements for 70% and 75% choline chloride aqueous solutions
Choline chloride content, %
Ethylene glycol content, %
Blue methylamine content, %
Heavy metal (as Pb) content, %
Test method
5.1 Identification test
5.1.1 Reagents and materials| |tt||5.1.1.1 Potassium hydroxide.
5.1.1.2 Potassium permanganate.
5.1.1.3 Sulfuric acid solution: 6+100.
5.1.1.4 Nitric acid solution: 10.5-100.
5.1.1.5 Chromium ammonium thiocyanate solution.
70% aqueous solution
Weigh 0.5g chromium ammonium thiocyanate, add 20mL water, shake for half an hour and filter. This solution cannot be used after 48 hours.
5.1.1.6 Potassium mercuric iodide solution.
75% aqueous solution
Weigh 1.36g mercuric chloride, add 60mL water to dissolve, and weigh 5g potassium iodide and add 10mL water to dissolve. Mix the two solutions and dilute to 100mL with water.
5.1.1.7 Ammonia solution: 4+10.
5.1.1.8 Silver nitrate solution: 17g/L.
5.1.1.9 Red litmus paper.
Take a filter paper strip and immerse it in litmus indicator solution. Add a very small amount of hydrochloric acid to make the filter paper strip red. Take it out and dry it in a shade for later use. The color change range is pH4.5～8.0 (red→blue).
5.1.1.10 Starch-potassium iodide test paper.
Instructions for use:
1) The "Summary of the Safety Laws and Regulations for Feed Additives" has a drying loss item. 187
5.1.2 Identification method
HG 2941- 1999
5.1.2.1 Weigh 0.5g of sample, add 50mL of water to dissolve, take 5mL of sample solution, add 3mL of ammonium chromium thiocyanate solution, and a red precipitate will be produced.
5.1.2.2 Weigh 0.5g of sample, add 10mL of water to dissolve, take 5mL of sample solution, add 2 drops of potassium mercuric iodide solution, and a light yellow precipitate will be produced.
5.1.2.3 Weigh 0.5g of sample, add 5mL of water to dissolve, add 2g of potassium hydroxide and several grains of potassium permanganate, and release ammonia when heated to turn the wetted red litmus paper blue.
5.1.2.4 The aqueous solution of the sample shows the identification reaction of chloride. Take an appropriate amount of sample, add ammonia solution to make it alkaline, divide it into two parts, add nitric acid solution to one part to make it acidic, add silver nitrate solution to produce white curd-like precipitate, the separated precipitate can be dissolved in ammonia solution, add nitric acid solution again, and the precipitate will be generated again; add sulfuric acid solution to the other part to make it acidic, add a few crystals of potassium permanganate, heat it to release chlorine gas, and make the starch-potassium iodide test paper appear blue.
5.2 Determination of choline chloride content (arbitration method) 5.2.1 Principle of the method
The content is determined by non-aqueous titration. Mercuric acetate is used to convert choline chloride into acetate and poorly ionized mercuric fluoride, and the resulting acetate is titrated with perchloric acid in an acetic acid medium. The reaction equation is as follows:
2[(CH.),NCH,CH,OHCI+Hg(CH,COO),CH:COOH,+2CH;COO(CH3);NCH,CH2OH+HgCl2HCIO4
CHCOOH
5.2.2 Reagents and materials
(CH:),NCH2CH2OHCIO. -+CH,COOH5.2.2.1 Glacial acetic acid: high-grade pure, purity greater than or equal to 99.6% (mass fraction). 5.2.2.2 Acetic anhydride.
5.2.2.3 Mercuric acetate solution: 50g/L. Weigh 5g of mercuric acetate and grind it into powder. Add 100mL of warm glacial acetic acid to dissolve it. This solution should be placed in a brown bottle and sealed.
5.2.2.4 Crystal violet indicator solution: 2g/L. Weigh 0.2g of crystal violet and add 100mL of glacial acetic acid. 5.2.2.5 Perchloric acid standard titration solution: c(HClO,) = 0.1mol/L. If the temperature during calibration is different from the temperature during use, recalibrate or use formula (1) to correct its concentration1. Co
Gi = 1+ 0. 0011(t to)
Wherein: 0.0011.---volume expansion coefficient of glacial acetic acid, 1/℃; ta—temperature during calibration, ℃;
t—-temperature during use, C;
co--concentration of perchloric acid standard titration solution during calibration, mol/L; concentration of pernitrogen acid standard titration solution during use, mol/L. 5.2.3 Instruments and equipment
25 mlL acid burette.
5.2.4 Analysis steps
Weigh about 0.3g sample (accurate to 0.0002g), add 20mL glacial acetic acid, 2ml acetic anhydride, 10ml mercuric acetate solution and two drops of crystal violet indicator solution, shake the hook. Titrate with perchloric acid standard titration solution until the solution turns pure blue, and perform a blank test at the same time. Instructions for use:
1) The "11th Law Compendium on Safety of Feed Additives" does not provide a temperature correction formula. 188
5.2.5 Expression of analytical results
HG 2941 1999
The choline chloride content (X,) expressed as mass fraction is calculated according to formula (2): X = cV-V)×0.139.6 × 100
Wherein: c--
actual concentration of perchloric acid standard titration solution, mol/l.; V---volume of perchloric acid standard titration solution consumed by the sample, mL; V-volume of perchloric acid standard titration solution consumed by the blank, mL. m-mass of the sample, g;
. (2)
0.1396The mass of choline chloride expressed in grams equivalent to 1.00mL perchloric acid standard titration solution [c(HCIO4)=1.000mol/L].
5.2.6 Allowable difference
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 0.2%. 5.3 Determination of pH value
Measure an appropriate amount of sample in a dry and clean beaker, and immerse the sample with a precision pH test paper in the range of 5.5 to 9.0. After the test paper is moistened, take it out and compare the color with the standard color plate, or use a pH meter to determine its pH value. 5.4 Determination of ethylene glycol content
5.4.1 Principle of the method
Periodic acid (or periodate) oxidizes ethylene glycol, and the generated iodic acid (or iodate) and excess periodic acid (or periodate) react with potassium iodide to release iodine. Titrate iodine with sodium thiosulfate standard titration solution. The ethylene glycol content is obtained by the difference between the sodium thiosulfate standard titration solution consumed in the blank test and the sample test. Taking potassium iodate as an example, the reaction equation is as follows: KIO+C,H(OH)2 -→2HCHO+KIO,+HC KIO,+7KI+4H2SO —→4K,SO +412+4H,OK10:+5KI+3H,SO →3K,SO +312+3H,0I2+2Na2S,O; 2Nal +NazS,O
5.4.2 Reagents and materials
5.4.2.1 Potassium iodide.
5.4.2.2 Potassium periodate (or sodium) solution: 4g/1. 5.4.2.3 Sulfuric acid solution: 1+20.
5.4.2.4 Sodium thiosulfate standard titration solution: c(NazS,O,)=0.1 mol/L5.4.2.5 Starch indicator solution: 5g/L.
5.4.3 Analysis steps
Weigh about 4.5g of sample (if the ethylene glycol content in the sample is low, it can be increased as appropriate, accurate to 0.0002g), put it in a 250mL iodine volume flask, add 25.0mL potassium periodate (or sodium) solution, add 25mL sulfuric acid solution, and place it in the dark at room temperature for 30min. Add 50mL of water, then add 2g of solid potassium iodide, shake the hook, and immediately titrate with sodium thiosulfate standard titration solution until the solution is light yellow, add 1mL of starch indicator solution, and continue to titrate until the solution is colorless, which is the end point.
Conduct a blank test at the same time.
5.4.4 Expression of analysis results
The ethylene glycol content (X,) expressed as mass fraction is calculated according to formula (3): X - V/-V2) × 0. 031 04 × 100ml
Wherein: C.--actual concentration of sodium thiosulfate standard titration solution, mol/L.; volume of sodium thiosulfate standard titration solution consumed by the air, mL; V_
HG 2941 1999
volume of sodium thiosulfate standard titration solution consumed by the sample, mL; V
mass of sample, g;
0.03104—=mass of ethylene glycol in grams equivalent to 1.00mL of sodium thiosulfate standard titration solution [c(NazS,O:)=1.000mol/L].
5.4.5 Allowable difference
The arithmetic mean of the results of two parallel determinations shall be taken as the determination result. The difference between the results of two parallel determinations shall not be greater than 0.03%. 5.5 Determination of trimethylamine content
5.5.1 Principle of the method
Amine and picric acid react to generate a characteristic reaction of yellow picric acid trimethylamine salt, and the spectrophotometric method is used for quantitative determination. 5.5.2 Reagents and materials
5.5.2.1 Anhydrous sodium sulfate.
5.5.2.2 Toluene (anhydrous). Take 100ml of toluene in a separatory funnel and wash it three times with 1+35 sulfuric acid solution, 50ml each time, discard the sulfuric acid washing solution, add 20g of anhydrous sodium sulfate to dehydrate, dry it, and set it aside. 5.5.2.3 Saturated potassium carbonate solution.
5.5.2.4 Magnesium carbonate formaldehyde solution. Take 200ml of 36%~38% formaldehyde, add 20~30g of magnesium carbonate, and shake for 3min. Filter with filter paper, take 50ml of filtrate, and dilute with water to 500ml. 5.5.2.5 Picric acid toluene solution.
Reserve solution: weigh 1g of picric acid that has been dried in a desiccator in advance, and dissolve it in 50ml of anhydrous toluene. Working solution: take 1mL of reserve solution and dilute with anhydrous toluene to 100mL. 5.5.2.6 Trimethylamine standard solution. Weigh (0.0810±0.0001)g of trimethylamine hydrochloride that has been dried at 105℃ for 4h, dissolve it in a 100ml volumetric flask with water, take 10mL, add it to a 250mL volumetric flask, and dilute with water to the mark. This solution contains 20μg of trimethylamine in 1mL. 5.5.3 Instruments and equipment
Spectrophotometer,
5.5.4 Analysis steps
5.5.4.1 Drawing of working curve
Put 0.0, 1.0, 2.0, 3.0, 4.0, and 5.0 mL of 20μg/mL trimethylamine standard solution into a 125ml separatory funnel, fill the volume to 5mL with water, add 1mL magnesium carbonate formaldehyde solution, 10.0mL toluene, and 3mL saturated potassium carbonate solution, shake vigorously for 1min, and let stand for 5min. Transfer each toluene layer into a covered test tube containing 0.5g anhydrous sodium sulfate, and dehydrate. Take 5.0ml of this solution, add 5.0mL picric acid toluene solution, and mix well. Colorimetric at a wavelength of 410nm. Use 1cm colorimetric blood and the reagent blank as the reference solution to measure its absorbance.
Use trimethylamine content as the horizontal axis and absorbance value as the vertical axis to draw a working curve (calibrate once a quarter). 5.5.4.2 Determination of sample
Weigh 1g of sample (if the trimethylamine content is low, it can be increased appropriately, accurate to 0.0002g), place it in a 50mL volumetric flask, dilute with water to the scale, mix well, and take 5.0mL is placed in a 125mL separatory funnel, and 5mL of water is taken for blank test. The following operation is the same as the drawing of the working curve, and the reagent blank is used as the reference solution.
The measured sample absorbance value is checked against the working curve to find the corresponding trimethylamine content. 5.5.5 Expression of analysis results
The trimethylamine content (X3) expressed as mass fraction is calculated according to formula (4): X, =
To use explanation:
mo× 10-3
1"Japanese Feed Additive Safety Law Summary" adopts the self-viewing limit colorimetric method. 190
HG 2941 --- 1999
Where: m--trimethylamine content found from the working curve, ug; mz--mass of a sample, g.
5.5.6 Allowable difference
Take the arithmetic mean of the results of two parallel determinations as the determination result. The relative deviation of the results of two parallel determinations shall not exceed 10%. 5.6 Determination of ash content
5.6.1 Reagents and materials
5.6.1.1 Sulfuric acid.
5.6.1.2 Hydrochloric acid solution: 1+1.
5.6.2 Instruments and equipment
High temperature furnace (1000±10)℃.
5.6.3 Analysis steps
Soak the porcelain crucible in hydrochloric acid solution for 24h, wash and dry. Weigh 2g of sample (accurate to 0.0002g) and place it in a constant mass molten iron at 800℃. Add 0.5mL of sulfuric acid and slowly heat it on an electric furnace until the sample is completely carbonized, then move it into a high temperature furnace and burn it at 800℃ for 2h. Take out the crucible and cool it in the air for 1~3min, move it into a desiccator and cool it to room temperature, and weigh it until the mass is constant. 5.6.4 Expression of analysis results
The ash content (X) expressed as mass fraction is calculated according to formula (5): X,=ms=m× 100
Wherein: m-mass of added residue, g;
m.----mass of crucible, g;
--mass of sample, g.
5.6.5 Allowable difference
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 0.02%. 5.7 Determination of heavy metal content
5.7.1 Principle of the method
Under weakly acidic conditions, the heavy metals in the sample react with sodium sulfide to form brown-black precipitates, which are turbidized with the lead standard solution treated in the same way and subjected to limit test.
5.7.2 Reagents and materials
5.7.2.1 Acetic acid solution: 60g/L.
5.7.2.2 Sodium sulfide solution: 50g/L. Re-prepare when the solution changes color or becomes turbid. 5.7.2.3 Lead standard solution: 0.01mg lead per ml. Take 10mL of lead standard solution containing 0.1mg lead per ml in a 100mL volumetric flask and dilute to scale.
5.7.3 Analysis steps
Weigh (1.00±0.01)g of the sample and dissolve it in 40mL of water. Transfer the solution into a 50mL colorimetric tube, add 2mL of acetic acid solution, and dilute with water to the scale to obtain the sample solution.
In another colorimetric tube, add 2mL of lead standard solution, dissolve it in 40mL of water, add 2mL of acetic acid solution, and dilute with water to the scale to obtain the standard colorimetric solution.
Add 1 drop of sodium sulfide solution to each of the sample solution and the standard colorimetric solution, mix well, and place in a dark place for 5min. Observe from top to bottom against a white background. The dark turbidity of the sample solution should not be darker than the standard colorimetric solution. 6 Inspection rules
6.1 70% and 75% choline chloride aqueous solution should be inspected by the quality inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer should ensure that all products shipped out of the factory meet the requirements of this standard. HG 2941-1999
Each batch of products shipped out of the factory must be accompanied by a product quality inspection certificate that complies with this standard, including: product name, production batch number or expiration date, net content, shelf life, this standard number, production license number, manufacturer name and address. 6.2 The amount of product produced by each kettle at one time is considered a batch. 6.3 Determine the number of sampling units in accordance with the provisions of 6.6 in B/T6678-1986. When sampling, shake the product evenly and use a clean and dry open sampling tube to sample from the full liquid level in the container. That is, slowly put the sampling tube into the liquid so that the liquid levels inside and outside the tube are kept at the same level. When it reaches the bottom, close the upper end of the tube, pull out the sampling tube, and put the collected sample into a clean, dry, stoppered glass bottle. The sampling volume of each barrel shall not be less than 100g. Mix the sample thoroughly. Take out 500g from it and divide it into two clean, dry, ground-stoppered glass bottles, affix labels and indicate: manufacturer name, product name, production batch number, sampling date and sampler name. One bottle is for inspection, and one bottle is sealed and stored for reference in two months. 6.4 Determination of test results
6.4.1 If one of the indicators in the test results does not meet the requirements of this standard, re-sample from twice the amount of packaging for re-inspection. Even if only one indicator of the re-inspection result does not meet the requirements of this standard. The entire batch of products is unqualified. 6.4.2 The final expression of the analysis results shall be consistent with the number of digits required in Table 1. 7 Label, packaging, transportation and storage
7.1 The label on the packaging barrel of this product shall comply with the provisions of GB10648. 7.2 Feed grade choline chloride aqueous solution can be packaged in galvanized iron barrels or polyethylene plastic barrels, with a net content of (200±1) kg, (100±0.5) kg per barrel, or packaged according to user requirements. 7.3 Prevent damage during transportation, and do not mix with toxic substances. 7.4 This product should be stored in a dry, sealed, and light-proof place. The shelf life is 24 months. Part II 50%, 60% choline nitride powder
8 Requirements
8.1 Properties
This product is a white or yellowish brown (depending on the excipient) dry flowable powder or granules, hygroscopic, with a specific odor. 8.250%, 60% choline nitride powder should meet the requirements of Table 2 1. Table 2 Requirements for 50% and 60% choline chloride powders
Choline chloride content (on a dry basis)
Loss on drying
Fineness (through 800um sieve)
9 Test method
9.1 Identification test
9.1.1 Reagents and materials
5.1.1.
9.1.2 Identification method
50% powder
Use instructions:
1) The "Compendium of Safety Laws and Regulations for Feed Additives" does not set items for loss on drying and fineness. 192
60% powder
HG 2941 1999
Weigh 2g of the sample, add 20mL of distilled water to dissolve, filter, and discard the residue. Identify using the identification method specified in 5.1.2. 9.2 Determination of Choline Chloride Content
9.2.1 Principle of the Method
The choline chloride contained in the sample is extracted with methanol. After evaporating the solvent, the choline chloride content is determined by non-aqueous titration.
9.2.2 Reagents and Materials
9.2.2.1 Methanol.
9.2.2.2 Other reagents and materials are the same as in 5.2.2. 9.2.3 Instruments and Equipment
25mL acid burette.
9.2.4 Analysis steps
Weigh 0.7g of the sample dried at 105℃ to a constant mass (0.6g of 60%, accurate to 0.0002g), place it in a 250mL conical flask, add 40mL of methanol, shake it thoroughly for 30min and filter it. Then wash the precipitate three times with 20, 15 and 15mL of methanol respectively. Combine the filtrate and washing liquid, evaporate it to dryness on a water bath to obtain dry residue A. Heat and dissolve the dry residue A with 20mL of glacial acetic acid, and then perform the analysis according to the analysis steps specified in 5.2.4. Perform a blank test at the same time.
9.2.5 Expression of analysis results
Perform according to the provisions of 5.2.5.
9.2.6 Allowable difference
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 0.5%. 9.3 Determination of loss on drying
9.3.1 Analysis steps
Weigh about 4g of sample (accurate to 0.0002g), place it in a weighing bottle that has been dried at 105℃ to constant mass, and put it in a constant temperature drying oven at 105℃ for 2h. Move it into a desiccator to cool to room temperature and weigh it until the mass is constant. 9.3.2 Expression of analysis resultsbzxZ.net
The loss on drying (X.) expressed as mass fraction is calculated according to formula (6): Xs= mo= m ×100
Where: m: mass of the sample plus the weighing bottle before drying, g; m-mass of the sample plus the weighing bottle after drying, g; -mass of the sample, g.
9.3.3 Allowable difference
Take the arithmetic mean of the results of two parallel measurements as the measurement result. The difference between the results of two parallel measurements shall not be greater than 0.2%. 9.4 Determination of fineness
9.4.1 Principle of the method
Use a test sieve of specified mesh to sieve a known amount of sample, and measure the mass passing through the test sieve to express its fineness. 9.4.2 Instruments and equipment
Test sieve: 800μm.
9.4.3 Analysis steps
Weigh about 10g of sample (accurate to 0.01g), place it on the test sieve for sieving, and weigh the material under the sieve (accurate to 0.01g). 9.4.4 Expression of analysis results
The mass of the sample passing through the test sieve expressed as mass fraction (X.) is calculated according to formula (7):.(6)
Where: mio--
The mass of the sample passing through the test sieve·g;
The mass of the sample, g.
9.4.5 Allowable difference
HG2941
—1999
X. = mlo× 100
Take the arithmetic mean of the results of two parallel determinations as the determination result. The difference between the two parallel determination results shall not be greater than 1%. 10 Inspection rules
10.150%, 60% choline chloride powder shall comply with the provisions of 6.1. 10.2 Product quantity per batch: intermittent drying process is calculated as one swatch; continuous drying process is calculated as one production shift. 10.3 Determine the number of sampling units according to 6.6 of GB/T6678--1986. When sampling, use a sampler to vertically insert the sample into the center of the bag mouth at three-quarters of the depth. The sampling quantity of each bag shall not be less than 100g. Mix the sample thoroughly, divide it into quarters to not less than 500g, and pack it into two clean, dry glass bottles with ground stoppers. Label them and indicate: manufacturer name, product name, production batch number, sampling date and name of the sampler. One bottle is for inspection, and the other is sealed and stored for two months for reference.
10.4 The determination and expression of the test results are the same as those in 6.5. 11 Labeling, packaging, transportation and storage
11.1 Labels should comply with GB10648.
11.2 Feed grade choline fluoride powder is quantitatively packaged in non-toxic plastic bags inside and paper plastic bags outside. The packaging bag should be accompanied by a product instruction manual. The net content of each bag is 25kg, 20kg, or packaged according to user requirements. 11.3 During transportation, cover should be used to prevent sun exposure or rain, and it should not be mixed with toxic items to prevent packaging damage. 11.4 This product should be stored in a dry, cool and ventilated warehouse. The shelf life is 18 months. 194
HG 2941 —1999
Appendix A
(Appendix to the standard)
Determination of Choline Chloride Content
Argentometric Method (Mole Method)
When this method is used to determine the content of choline chloride, it must be calibrated by non-aqueous titration before use. A1 Determination of Aminated Choline Content in 70% and 75% Choline Chloride Aqueous Solutions A1.1 Principle of the Method
This method determines the content of choline fluoride by analyzing the chlorine content in the sample. Potassium chromate is used as an indicator when detecting chloride ions. According to the difference in solubility between silver chloride and silver chromate (the solubility of silver chloride is less than that of silver chromate), fluoride ions are titrated with silver nitrate. When brick-red silver chromate precipitate begins to precipitate, it is the end point.
A1.2 Reagents and Materials
A1.2.1 Standard silver nitrate titration solution: c(AgNO,)=0.1 mol/L. A1.2.2 Potassium chromate indicator solution: 100g/L. A1.3 Analysis Steps
Weigh 0.5g of the sample (accurate to 0.0002g), place it in a 250mL iodine volumetric flask, add 50mL of water and shake well, then add 0.5mL of potassium chromate indicator solution, and titrate with standard silver nitrate titration solution until it turns brick red, which is the end point. Perform a blank test at the same time.
A1.4 Expression of analysis results
The choline fluoride content (X,) expressed as mass fraction is calculated according to formula (A1): X, = 2(VV) × 0. 139 6 × 100mn
Wherein: C2—actual concentration of silver nitrate standard titration solution, mol/L; Va——volume of silver nitrate standard titration solution consumed by the sample, mL; V3—volume of silver nitrate standard titration solution consumed by the blank test, ml. (A1))
m Mass of sample, g;
0.1396---mass of choline chloride expressed in grams equivalent to 1.00mL silver nitrate standard titration solution Lc(AgNO,)=1.000mol/L].
A1.5 Allowable difference
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 0.2%. A2 Determination of choline chloride content in 50% and 60% choline chloride powders A2.1 Principle of the method
The choline chloride contained in the sample is dissolved in water, and the filtrate is filtered and the choline chloride content is determined by the silver method (Mohr method). A2.2 Reagents and materials
Same as A1.2.
A2.3 Analysis steps
Weigh 1.4g (1.2g for 60%, accurate to 0.0002g) of the sample dried at 105℃ to a constant mass and place it in a 100mL volumetric flask, add water to dilute to the scale, shake well, and leave for 20min. Filter, discard about 20ml of the initial filtrate. Accurately measure 50.0ml of the subsequent filtrate, put it in a conical flask, add 0.5mL of potassium chromate indicator solution, and proceed as specified in A1.3. 195
HG2941 -1999
At the same time, use the excipients of this batch of products for blank test. A2.4 Expression of analysis results
Same as A1.4.
A2.5 Allowable difference
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 0.5%. 1961 Principle of the method
This method determines the content of choline fluoride by analyzing the chlorine content in the sample. Potassium chromate is used as an indicator to detect chloride ions. According to the difference in solubility between silver chloride and silver chromate (the solubility of silver chloride is less than that of silver chromate), silver nitrate is used to titrate fluoride ions. When brick-red silver chromate precipitate begins to precipitate, it is the end point.
A1.2 Reagents and materials
A1.2.1 Standard silver nitrate titration solution: c(AgNO,)=0.1 mol/L. A1.2.2 Potassium chromate indicator solution: 100g/L. A1.3 Analysis steps
Weigh 0.5g of the sample (accurate to 0.0002g), place it in a 250mL iodine volumetric flask, add 50mL of water and shake well, then add 0.5mL of potassium chromate indicator solution, and titrate with standard silver nitrate titration solution until it turns brick red, which is the end point. Perform a blank test at the same time.
A1.4 Expression of analysis results
The choline fluoride content (X,) expressed as mass fraction is calculated according to formula (A1): X, = 2(VV) × 0. 139 6 × 100mn
Wherein: C2—actual concentration of silver nitrate standard titration solution, mol/L; Va——volume of silver nitrate standard titration solution consumed by the sample, mL; V3—volume of silver nitrate standard titration solution consumed by the blank test, ml. (A1))
m Mass of sample, g;
0.1396---mass of choline chloride expressed in grams equivalent to 1.00mL silver nitrate standard titration solution Lc(AgNO,)=1.000mol/L].
A1.5 Allowable difference
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 0.2%. A2 Determination of choline chloride content in 50% and 60% choline chloride powders A2.1 Principle of the method
The choline chloride contained in the sample is dissolved in water, and the filtrate is filtered and the choline chloride content is determined by the silver method (Mohr method). A2.2 Reagents and materials
Same as A1.2.
A2.3 Analysis steps
Weigh 1.4g (1.2g for 60%, accurate to 0.0002g) of the sample dried at 105℃ to a constant mass and place it in a 100mL volumetric flask, add water to dilute to the scale, shake well, and leave for 20min. Filter, discard about 20ml of the initial filtrate. Accurately measure 50.0ml of the subsequent filtrate, put it in a conical flask, add 0.5mL of potassium chromate indicator solution, and proceed as specified in A1.3. 195
HG2941 -1999
At the same time, use the excipients of this batch of products for blank test. A2.4 Expression of analysis results
Same as A1.4.
A2.5 Allowable difference
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 0.5%. 1961 Principle of the method
This method determines the content of choline fluoride by analyzing the chlorine content in the sample. Potassium chromate is used as an indicator to detect chloride ions. According to the difference in solubility between silver chloride and silver chromate (the solubility of silver chloride is less than that of silver chromate), silver nitrate is used to titrate fluoride ions. When brick-red silver chromate precipitate begins to precipitate, it is the end point.
A1.2 Reagents and materials
A1.2.1 Standard silver nitrate titration solution: c(AgNO,)=0.1 mol/L. A1.2.2 Potassium chromate indicator solution: 100g/L. A1.3 Analysis steps
Weigh 0.5g of the sample (accurate to 0.0002g), place it in a 250mL iodine volumetric flask, add 50mL of water and shake well, then add 0.5mL of potassium chromate indicator solution, and titrate with standard silver nitrate titration solution until it turns brick red, which is the end point. Perform a blank test at the same time.
A1.4 Expression of analysis results
The choline fluoride content (X,) expressed as mass fraction is calculated according to formula (A1): X, = 2(VV) × 0. 139 6 × 100mn
Wherein: C2—actual concentration of silver nitrate standard titration solution, mol/L; Va——volume of silver nitrate standard titration solution consumed by the sample, mL; V3—volume of silver nitrate standard titration solution consumed by the blank test, ml. (A1))
m Mass of sample, g;
0.1396---mass of choline chloride expressed in grams equivalent to 1.00mL silver nitrate standard titration solution Lc(AgNO,)=1.000mol/L].
A1.5 Allowable difference
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 0.2%. A2 Determination of choline chloride content in 50% and 60% choline chloride powders A2.1 Principle of the method
The choline chloride contained in the sample is dissolved in water, and the filtrate is filtered and the choline chloride content is determined by the silver method (Mohr method). A2.2 Reagents and materials
Same as A1.2.
A2.3 Analysis steps
Weigh 1.4g (1.2g for 60%, accurate to 0.0002g) of the sample dried at 105℃ to a constant mass and place it in a 100mL volumetric flask, add water to dilute to the scale, shake well, and leave for 20min. Filter, discard about 20ml of the initial filtrate. Accurately measure 50.0ml of the subsequent filtrate, put it in a conical flask, add 0.5mL of potassium chromate indicator solution, and proceed as specified in A1.3. 195
HG2941 -1999
At the same time, use the excipients of this batch of products for blank test. A2.4 Expression of analysis results
Same as A1.4.
A2.5 Allowable difference
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 0.5%. 196
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