Some standard content:
ICS65.120
Agricultural Industry Standard of the People's Republic of China
NY/T 723—2003
Feed Grade
Potassium iodate for feed
2003-12-01 Issued
Ministry of Agriculture of the People's Republic of China
2004-03-01 Implementation
NY/T723-2003
Standard for Potassium Iodide for Feed Grade is based on the standards and documents such as the Codex Alimentarius of the United States (F. (1996 Edition) and is formulated through a large number of experimental studies
This standard is proposed by the Market Economy and Information Department of the Ministry of Agriculture. This standard is drafted by the Animal Husbandry and Veterinary Bureau of the Ministry of Agriculture. This standard is drafted by the Food Quality Supervision and Inspection and Testing Center (Xi'an) of the Ministry of Agriculture. The main drafters of this standard are: Hu Guixiang, Li Sheng, Li Huileng, Zhao Caihui, Chen Li, Han Yongjian, Yao Junhu. 1 Scope
Feed Grade Potassium Iodide
NY/T 723—2003
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of feed-grade potassium iodate. This standard applies to feed-grade potassium iodate produced by potassium chlorate oxidation method, etc. This product is added to feed as an iodine supplement. 2
Normative references
The clauses in the following documents become the signature of this standard through the application of this standard. For any dated reference, all subsequent amendments (excluding errata) or revisions do not apply to this standard. However, the parties to the agreement on this standard are encouraged to consider whether the latest versions of these documents can be used. For any undated reference, the latest version of the document shall apply to this standard. Preparation of standard solutions for titration analysis (quantitative analysis) of chemical reagents GB/T 601
GB/r 602
Preparation of standard solutions for determination of impurities in chemical reagents Preparation of preparations and products used in test methods for chemical reagents GB/T 604
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 605
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 606
Preparation of preparations and products used in test methods for chemical reagents GB/T 607
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 608
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 609
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 610
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 611
Preparation of standard solutions for determination of impurities in chemical reagents GB/T 612 G03
GB/T 6435
Determination method of moisture in feed
G1313848 Feed standard
CB/T14689.=Feed sampling method
3 Requirements
3.1 Appearance and properties
This product is colorless or white powder, odorless, soluble in water, difficult to dissolve in ethanol, the pH value of the sample aqueous solution (1+20) is 5.~7.℃3.2 Technical indicators
The technical indicators should meet the requirements of Table 1.
Table 1 Technical indicators
Indicator name
Iodic acid ()
Potassium iodate (in terms of)
Total (As)
Heavy metals (in terms of Pbs)
Nitric acid salts
Dry tip weight
4 Test method
. o: s
The reagents, water and instruments used in this standard, unless otherwise specified, are analytically pure reagents and distilled water of high purity, and are placed in general laboratory instruments.
Standard solutions, impurity standard solutions, preparations and products required for determination, unless other standards are specified, are prepared in accordance with the provisions of (3/1601GB/T6C2 and GB/T603
Safety Tips: Some strong acids are required in the test operation of this standard, so be careful to avoid splashing on the skin: When using volatile reagents, they must be carried out in a fume hood.
4.1 Appearance and properties
Sensory evaluation should meet the requirements of 3.1.
4.2 pH determination
4.2.1 Instruments and equipment
Acidometer.
4.2.2 Determination method
Weigh 1g (accurate to 0.01g): place in a 50ml beaker, add 20mL of water to dissolve, and use an acidometer to measure its pH value to 5. 0~-7. 0,
4.3 Identification
4.3.1 Reagents and solutions
4. 3. 1. 1 Lack of acid.
4.3.1.2 Phosphorous acid solution (1 + 4)
4.3.1.3 Powder indicator solution: Take 0.5g of soluble starch and add 5ml of water. Stir well, slowly pour in 10ml of boiling water +. Stir occasionally until it is translucent, and take the upper clear layer. 4.3.2 Identification method
4.3.2.1 Weigh 1g of this product and dissolve it in 20ml of water. Take 1 ml of the test solution, add two drops of starch indicator and a few drops of phosphorous acid solution (4. 3. 1. 2), which turns blue
4.3.2.2 Take a platinum wire, moisten it with hydrochloric acid, and burn it in a colorless flame until it turns colorless. Take a sample: burn it in a colorless flame, the flame will turn purple, and when it contains the least sodium salt, it can be identified by looking under a blue glass. 4.4 Determination of potassium iodate
4.4.1 Principle
In an acidic solution, iodate ions are reduced to free iodine by iodide ions. Then titrate with sodium thiosulfate standard solution. Sodium thiosulfate reduces free iodine to iodine ions. Starch solution is used as the indicator solution, and the end point of the reaction is determined by the color change. 4.4.2 Reagents and solutions
4.4.2.1 Potassium hydroxide,
4. 4.2.2 Solution: (1+4).
Powder indicator solution: Prepare according to 4.3.1.3.
4. 4. 2. 3
4.4.2.4 Sodium thiosulfate standard titration solution: r(NaS(),) is about C.nol/L4. 4.3 Determination method
Weigh 0.8g of sample, weigh to 0.00C1g, put it in a 250mL volumetric flask, add water to dissolve and dilute to the scale, shake. Transfer 25.00ml. Put it in an iodine volumetric flask. Add 2g potassium iodide and 10ml hydrochloric acid solution, then put it in a clear place for 5min, add 10ml water. Titrate with sodium thiosulfate standard titration solution (4.4.2.4). When it is close to the end point, add 2IiL starch indicator solution and continue titrating until the monitor disappears. This is the end point. Perform a blank test at the same time.
4. 4.4 Calculation of analysis results
The content of potassium iodate expressed as mass fraction (calculated as K1C) is calculated according to formula (1): x =tV-Ve)X0 035 67 ×100= s(Vv.)×35. 67mx
The content of potassium iodate (calculated as I) expressed as mass fraction is calculated according to formula (2): x; - (V Vo) ×0 021 15 × 100 = c(VY) × 21. 15m×250
Wu Zhong:
X.--the content of potassium iodate (in KIO4) in the sample; x, the content of iodic acid (in iodine) in the sample; concentration of standard titration solution of sodium thiosulfate - in milliliters (n:1/:AY/1723-2003
V--the volume of standard titration solution of sodium thiosulfate consumed in titration of test solution, in milliliters (n:1): V\-the volume of standard titration solution of sodium thiosulfate consumed in titration of blank test Solution volume. Unit is ml; Sample mass. Unit is gram ();
2.03567——Mass of potassium iodate (K10,) expressed in grams equivalent to 1.00ml. sodium thiosulfate standard titration solution, c (Na:% 0.) = 1.00mol1:
0.021! 1.00ml sodium thiosulfate standard titration solution aS) 1.03mol11. The pressure of iodine (1) expressed in grams.
4. 4.5 Result expression
The average value of the results of the parallel determinations is the determination result, and the result is expressed to the decimal place. The deviation is not more than 1. 4.5 Determination of arsenic content (silver salt method) wwW.bzxz.Net
4.5.1 Method summary
The sample is digested with acid and potassium iodide and stannous chloride are used to reduce the high-valent species to ":" valent species. Then the new hydrogen generated by the reaction is absorbed by the silver salt solution to form a brown-red complex. The H absorbance is measured by spectrophotometry at a wavelength of 2211. 4.5.2 Reagents and solutions
4.5.2.1 Acid
4.5.2.2 High chloride
4.5.2.3
Sulfur solution (1 + 1)
4.5.2.4
4. 5. 2. 5
Nitric acid,
"Methyl chloride.
4. 5.2. 6
Zinc particles without base.
Potassium iodide solution: 15cg/L. 150g potassium iodide is dissolved in water and the volume is made up to 1ml. Store in a brown bottle. 4. 5.2.7
Stannic chloride solution: 100g/1.200)g tin fluoride SmC·2H. (make up to 100ml. concentrated hydrochloric acid. 4. 5. 2.8
Hydrochloric acid solution: 1 mol/l, take 81 ml of hydrochloric acid. Add water to 4 ml. 5. 2. 9
4.5.2.10 Lead acetate dilution: Soak cotton wool in 10/[10] acid solution for about 1 hour. Remove the residual liquid, dry it naturally or store it in a sealed bottle at 000℃.
4.5.2.11 Arsenic absorption solution: Diethylamino-silver thiosulfate (Ag-3J): 0.5 ethylamine-chloroform absorption solution: 1. Weigh 2.5g (accurate to 0.0002g) at 100℃ in a dry beaker. Add appropriate amount of chloroform to dissolve the gold. Transfer it to a 1030ml.7 volumetric flask, add 2m amine and make up to volume with trichloroethane. Put the subscript in the middle and place it in a cold place. Long-term precipitation should be treated after the trip Fuchuan 4.5.2.12 standard stock solutions: 1.0 mgml. Accurately weigh 0.660 0 5 oxidation two kinds 1! %. Add 200g sodium hydroxide solution to dissolve it, then add 60ml sulfuric acid solution (1.3 ml). Make up to 1.00mg arsenic per ml: 4.5.2.131.0/ml 1. Standard T for dissolving: Accurately pipette 7.3) n: 1. Weigh 1.0% standard stock solution 1: 1: 2% water, the solution contains arsenic g || tt || standard can absorb up to 50)gml. Arsenic standard solution ml: 1.0/ml. Put it into the volumetric bottle, the solution can absorb 0.0/m: || tt || 4.5.3 Instruments and equipment || tt || 4.5.3.1 Spectrophotometer || tt || 4.5.3.2 Arsenic absorption test: 1NY/T 723--2003
中35·~中央34
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碎化氧创器；
2气导管，
3-ABSORBER，
Lead acetate cotton
4. 5. 4 Measurement steps
4.5.4.1 Sample treatment
16±*0. 5
Figure 1 Arsenic generation and absorption device
Weigh 3g~5 of sample (accurate to 0.0C1) in a 250ml one-corner bottle, add a little water to moisten the sample, then add 20ml nitric acid, 5ml sulfuric acid, insert a funnel into bottle I, let it stand for 4 hours, add 5ml Perchloric acid, place on heating plate L for digestion. As the digestion time increases, the temperature gradually increases. When the digestion liquid turns purple and emits purple gas, continue to increase the temperature for digestion until the digestion liquid in the bottle turns completely white, then remove it, cool it, apply 1Ctnl.1 mnl/1. hydrochloric acid solution to boil and dissolve, cool it and transfer it to a 50 ml volumetric plate, add water to the scale, shake it for testing, and prepare the reagent blank solution at the same time.
4.5.4.2 Drawing of standard curve
Accurately pipette arsenic standard solution (1, 0 ug/mL) 0. 00 mL, t. 00 ml, 2. 00 mL, 4. 00 inl.. 6. 00) ml.VY/ 723-2003
S.00ml. Place the aliquots in the chain of the arsenic generator and add 4ml of water. Add 10ml of sulfuric acid solution. 1ml of potassium iodide solution (4.3.2.7). Shake well. 1ml of stannous chloride dissolved in iridium (4.5.2.8). Shake well. Let stand for 15min. Add 3 zinc granules, and gradually insert a gas guide tube filled with lead acetate cotton into the liquid chamber of a graduated test tube containing 5ml of absorption liquid, so that the generated arsenic oxide is absorbed into the absorption liquid. React at room temperature for 45 minutes, remove the absorption tube, add trichloroethane and ml.. probe, and pour the solution into a 1cm colorimetric tube. Measure the absorbance at a wavelength of 522nm. With the content of the species as the horizontal axis and the absorbance as the vertical axis, draw a standard curve. 4.5.4.3 Sample determination
Accurately absorb a certain amount of sample digestion solution (4.5.4.1) and reagent blank solution into the conical bottle of the arsenic generator, add 40ml of water... Follow the steps of drawing the standard curve, measure the corresponding absorbance, and compare it with the standard curve to determine the content of the species in the sample. 4.5.5 Determination results
4.5.5.1 Calculation formula
The arsenic content expressed as mass fraction (%) is calculated according to formula (3): XA. Vi (m.-m.)
Wherein:
The content of arsenic in the sample. x 10 4
m:---the mass of the sample digestion solution, in g (g);
V:---the total volume of the sample digestion solution, in milliliter (ml); V.
The volume of the sample digestion solution used for determination, in milliliter (ml); x 10 4
m:---the mass of the sample digestion solution used for determination, in microgram (g); m:
The mass of arsenic in the blank test sample, in microgram (g) 4. 5. 5. 2 Expression of results
The short sample is made into parallel samples, and the arithmetic mean value is taken as the analytical result. The result is expressed to two decimal places. When the amount of lead in each gram of sample is less than or equal to 1.0, the result shall be rounded to three significant figures. 5.5.3 Permissible deviation The relative deviation of the analysis result shall meet the requirements of Table 2. Table 2 requires that the amount of lead in each gram of sample should be less than or equal to 1.0 mg. 1-5.0 mg. 5.3. ~-10.90 mg. 4.6 Determination of lead content (by absorption spectroscopy) 4.6.1 Summary of the method Permissible deviation (length) After digestion, the sample is extracted and separated, and then introduced into an atomic absorption spectrophotometer. After atomization, the absorbance at the left side is measured. Compare with the standard series for determination. 4.6.2 Reagents and solutions 4.6.2.1 Nitric acid, 4.6.2.2 Sulfur. 4. 6.2.3 Perchloric acid.
4.6.2.4
Methyl isocyanate,
4.6.2.5 Acid solution: add to 4.2.9.4.6.2.62
Potassium iodide solution: concentration (KI) is 1 mmol/l: weigh 166 g potassium iodide: dissolve in 1:1 water, store in a brown bottle,
NY/T 723—2003
4.6.2.7 Ascorbic acid test solution: 50 mmol/l, weigh 5.0 g ascorbic acid, dissolve in water. Dilute to: 0.0 ml., stored in brown bottles. 4.6.2.8 Lead standard solution: 1.0/mL diluted with lead standard solution (1000/mL) 4.6.3 Instruments and equipment
4.6.3.1 Electron absorption spectrophotometer:
4.6.3.2 Lead hollow cathode lamp
4.6.4 Determination steps
4.6.4.1 Sample treatment
Transfer 5% of the sample (0.001 g) to a 2 ml conical flask, add a little water, filter the sample, then add 20 mL of caustic soda, 1 mL of sulfuric acid, place it on the bottle, and place it for 4 hours. Add 5 mL of perchloric acid, and place it on a hot plate for digestion. As the digestion time increases, the mixture is gradually heated until the digestion solution turns purple and the purple liquid is discharged, and the mixture is continued to be heated and digested. When the digestion solution in the bottle turns completely white, it is cooled. 1 ml hydrochloric acid solution: 1.2.9 boil to dissolve, transfer to 50 ml volumetric flask, add water to scale, remove and wait. Prepare the standard solution in the same way.
4.6. 4. 2 Plot the standard curve
Pipette 0 ml, 4 ml, 8 ml, 12 ml, 16 ml, 20 ml of the lead working solution (4.6. 2, 8) into a 5 mL volumetric flask, add 1 ml of water and add 2 ml potassium iodide solution (4.6.2. 6), shake: add 1 ml ascorbic acid solution (4.6.2. 7). Vibrate: accurately add 2 ml isobutyl ketone solution. Vigorously shake for 3 mm, let stand for 3 minutes, introduce the organic phase into the atomic absorption spectrophotometer, and measure the photometric value at 83.3 mm. Take absorbance as the vertical axis and lead content as the horizontal axis to draw a standard curve. 4.6.4.3 Sample determination
Accurately absorb 5ml. 10ml digestion solution and blank solution plus 25ml. in a flask. Determine according to the steps of drawing the standard line. Measure the absorbance value of the phase point and compare it with the standard curve for quantitative analysis. 4.6.5 Determination results
4.6.5.1 Calculation formula
The lead content expressed as a fraction by mass (%) is calculated according to formula (A): X
,
sample lead content:
sample mass, unit is g (kg):
total volume of sample digestion solution. Specific unit is liter (m.): ..... ..
The volume of the digestion solution of the test sample is measured in milliliters (ml): x1
The mass of lead in the digestion solution of the standard test sample is measured in micrograms (μg): The mass of lead in the blank test solution is measured in micrograms (μg), 4. 6.5. 2 Expression of results
Each sample should be analyzed in parallel, and the arithmetic mean is the analysis result. The result is expressed to two decimal places 4.6,5.3 Allowable error
The relative deviation of the analysis result should be derived from the requirements of Table 3 Table 3 Requirements
The content of lead in each dry potassium
.. G1 -.J5. 00
1.. t1...3, tm
. :0.
4.7 Determination of moisture
According to T4)
Six relative differences (yuan)
4.8 Determination of oxygenates
4.8.1 Reagents and materials: sulfuric acid.
NY/T 723-2003
4.8.2 Determination steps: Weigh 1.0g ± 0.1g sample. Put it into white porcelain and add 2ml sulfuric acid. Put it in a jar. The color should remain unchanged, and no color or gas should be generated.
5 Inspection rules
5.1 Factory inspection: The product should be inspected for loss on drying and main component content before leaving the factory. 5.2 Type inspection: All requirements specified in this standard are type inspection items. Type inspection shall be carried out when the product is put into production, raw materials are replaced, or supervised and inspected, or production is resumed after stopping production for more than half a year. 5.3 Feed grade potassium iodate shall be inspected by the quality inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a product certificate. 5.4 The user has the right to inspect and accept the received feed grade potassium iodate products in accordance with the provisions of this standard. 5.5 Sampling method: Implement in accordance with GB/T14699.1. 5.6 Judgment rule: If one of the indicators in the inspection results does not meet the requirements of this standard, double sampling shall be carried out for re-inspection. If one of the indicators in the re-inspection results still does not meet the requirements of this standard, the entire batch of products shall be judged as unqualified products. 6 Marking, packaging, transportation and storage
6. 1 Marking
The packaging shall have a warning symbol and the symbol "Do not directly contact the skin or eyes". Labeling
Labeling shall be implemented in accordance with GB10648.
6.2 Packaging
The packaging materials shall be packaged in brown or opaque plastic bags, wooden barrels lined with black plastic bags and sealed with thermoplastics, and the outer packaging shall be packaged in cartons, wooden boxes, and wooden barrels.
6.3 Transportation
During transportation, the products shall be covered to prevent sun and rain, and strictly prevent them from being knocked off to prevent the packaging materials from being damaged. It is strictly forbidden to transport them together with toxic and hazardous substances.
6.4 Storage
This product should be stored in a clean, ventilated, dry and cool place. It is strictly forbidden to mix with other stored items.
NY/T 723-2003
Agricultural Industry Standard of the People's Republic of China
Material Grade Potassium Iodate
NY/T 723--- 2003
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