Some standard content:
ICS65.080
Case number: F2432000
Chemical Industry Standard of the People's Republic of China
HG 32772000
Zinc sulfate for agricultural use
Zinc sulfate for agricultural use2000-05-23Promulgated
Implementation on 2000-12-01
Promulgated by the State Administration of Petroleum and Chemical Industry
HG3277—2000
This standard is revised from Chemical Industry Standard HG32771986t Zinc sulfate for agricultural use. The main differences between this standard and HG3277-1586 are: combined with the production conditions and capabilities of agricultural phthalate manufacturers in my country, according to the feedback from manufacturers, relevant quality supervision and inspection departments and users, more consideration is given to domestic and foreign standards, as well as GB/T12707.1991 Guidelines for Quality Comparison of Agricultural Products. Agricultural phthalates are divided into three categories: qualified, first-class and superior, and corresponding technical indicators are also specified. The problem of Fe2+ that cannot be removed by the original method when determining zinc content is solved, and the spectrophotometric method is added as the arbitration method for the determination of lead and carbon. The packaging logo and the selection method are also adjusted. From the date of implementation of this standard, the policies and regulations of the State Administration of Petroleum and Chemical Industry of the People's Republic of China can be put forward: This standard is under the jurisdiction of the National Fertilizer and Soil Treatment Agent Standardization Technical Committee. The responsible units for the development of this standard are: Shanghai Chemical Research Institute, Sichuan Fertilizer Quality Inspection Station. The main contributors of this standard are: Shang Zhaocong, Ji Hongman, and Zhang Tinghong. This standard was first issued in 1986.
1 Scope
Chemical Industry Standard of the People's Republic of China
Zinc Sulfate for Agricultural Use
Zine sultule Tur agricultural ugeJIG32772000
H32771985
This standard specifies the requirements, test methods, inspection specifications, certification, packaging, transportation and storage of zinc sulfate for agricultural use. This standard contains zinc sulfate monohydrate which is prepared by industrial acid reaction and is used as a trace element. The formula is: zinc sulfate monohydrate ZmS·H,
zinc sulfate heptahydrate ZmS·7H.O
molecular weight: zinc sulfate monohydrate 17.47 (according to 1995 international relative atomic mass): zinc sulfate heptahydrate 287.56 (according to 15 international relative atomic mass) 2 reference standards
The following provisions of the standard are excluded by reference in this standard. When this standard is published, the versions shown are valid and all standards will be maintained. All parties to the technical standards should use the following standards in case of possible new versions: B1-1930 Pictorial symbols for loading and unloading
GB/602--10% chemical reagent impurity determination method for filter drop (19053531.1962) Gn/12SC-999 Method for expressing limit values GR67R-1 General rules for sampling of industrial products in Hubei
GBGG79--1 98G Guben Chemical Products / 6821992 some room water specification test send e532: 1987 (1 version 3-1997 because of the heart of learning bar material || tt || GB/T17420-1238 micro 4 element rope material || tt || HG door 2543199Y fertilizer products chemical analysis commonly used standard titration solution, standard drop, reagent secretion indicator drop 3 product variety || tt || agricultural day economic acid according to the total number of water molecules contained in the product is divided into: 3.11 kinds contain one point 4.2 Requirements 4.1 Appearance: White or slightly yellow powder. 4.2 The use of the product should meet the requirements of Table 1. National Petroleum and Chemical Industry Bureau 200C-0523 approved 7000-12-01 implementation Zinc 2a1) Quality Index 1 S, measurement 5 Test Method H 3277-2000 Table 1 Requirements First-class product Zn, H4 Qualified product Superior product ZuSO, HC
Luger
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure water and the first-grade water specified in GBT6682. The liquids not specified in the above are all water-filtered, and the liquids to be determined are prepared with standard G/602. The liquids other than those specified in the above methods are prepared with 1G/T2.
5.1 Determination of zinc content FDTA coordination determination method 5.1.1 Method preparation
Add zinc fluoride (oxidized) and potassium iodide (in the presence of Fe2+, add hydrogen peroxide to oxidize Fe2+) to the zinc sulfoxide solution to eliminate the interference of the ions, and titrate with dimethyl orange as the indicator under the condition of HS~6 with disodium monoaminetetraacetic acid standard solution. The end point color is red to yellow.
5.1.2 Trial production materials
5.1.2.1 Non-normative.
5.1.2.2 Potassium iodide.
5.1.2.33% oxidizing solution.
Measure 50% overload effect 10ml and drop it into water, dilute to 1U1mL. 5.1.2.4 Acid solution 1+1
5.1.2.5 Six times neutralizing amine sea filter: 200g/5.1.2.6 Sodium iodide solution: 1g/.
The solution should be stored in a vinyl bottle after filtration
5.1.2.7 Potassium chloride solution: 103g/L
5.1.2.B Ethyl acetate solution: p15-65.1.2.9 Ammonia sample drop: 2g/L
5.1.2.10. Zinc acid-sodium EDTA) standard titration solution: cEDTA) 0.05mol/1.5.1.3 Titration
Weigh 2-%~3.U (accurate to .011) zinc sulfate or 4.~4.58 (0.001g) zinc sulfate, add enough water in a 250mL bottle, if the microfilm is mixed If the precipitate is turbid, add 1 μm sulfuric acid to acidify it. Dilute it with water and mix well. Put 1 μm test solution into a 25 μm beaker, add 50 ml of water, add potassium ferric oxide solution, if no blue precipitate is produced, test according to the method. If a blue precipitate is produced, continue the test by the method. Take 25.2 ml of test solution in 230 ml of beaker, boil water to 1 g ml, add 2 g of sodium chlorite and 1.5 g of potassium cyanide, add 1% dichloroethylene, then add tetramine dropwise until it turns yellow, add 10% sodium acetate buffer solution, and titrate with EDTA standard titration solution. The end point is when the solution changes from magenta to yellow. Note the consumption of EDTA standard titration solution.
HG32772000
b. Transfer 25.5mL of test sample into 250ml of solution. Add 2mL of hydrogen peroxide, mix well, heat in a ventilated chamber until it is slightly diluted and keep for 2min, cool immediately and then add acid solution until the solution becomes 100mT. Add 21mL of sodium iodide and 1g of iodide, then add a drop of methyl orange indicator solution, add six drops of tetramine solution until the solution turns red, add 10mL of sodium acetate, and titrate slowly with EIA standard solution. When the solution turns red again, check the solution with EDTA standard solution.
5.7.4 Analysis of the results
Use the mass fraction table to calculate (Zn) (X) Formula (1) Let X = 2Y.x0. Gi5 3Kx100
2m -250
The volume of FITA standard titration solution eliminated in the titration, the liquid concentration of 1.1-EDTA standard titration solution, 1.1/m sample mass 8
and 1.1.1.EDTA standard titration solution [eHITA = 1.00mol/. The mass of zinc in grams obtained by the parallel determination is taken as the determination result. 5-1.5 The absolute difference between the two parallel determinations is allowed to be no more than .20%. Do not return to the laboratory for measurement The cross-check of the results is not more than 0.30%. 5.2 Determination of free content by volumetric method
5.2.1 In the presence of a dry base methylene red mixed indicator solution, use sodium hydroxide standard to determine the free slow release in the sample. 5.2.2 Additives
5.2.2.1 Add water without carbon dioxide,
5.2-2H-2O-methyl red-methylene red mixed indicator solution (.1k methyl red in 50mL of % alcohol, then add.0 methylene chloride is removed and dissolved, then the sample is diluted with 1ml of alcohol.
5.2.7.3 Chloride oxidation standard solution (NmOH) (.1mbl/L) 5.2.3 Instruments and equipment
Microplate burette: 10mL:
5.2.4 Determination
Weigh about 1U (potential is C.01g> microneedle test, put it in a 150mL beaker, add 5Dml. water to dissolve. If the device can be tested, wash it with distilled water several times, collect the pool liquid and the sieve liquid in another beaker, add 1~drops of methyl red-isocyanate mixed indicator test solution, and use sodium hydroxide standard solution to determine until the color decreases to gray-green. The color is the color point, record the concentration of the standard titration solution of hydrogenation,
5.2.5 Expression of analytical parameters
The total amount of ionized acid (expressed as H2SO4) expressed as mass fraction (X,) is calculated according to formula (2): V1490x100
The concentration of the standard titration solution of sodium hydrogenation is 1.00mol/L
The mass of the acid expressed in grams equivalent to 1.00nL of the standard titration solution 1(N)H>=1.00mol/L
HG 3277—2000
The arithmetic pair of the parallel determination results shall be taken as the determination result. 5.2.6 The difference between the results of two parallel determinations shall be within the range of 1. The difference between the results of different experimental rates shall not be greater than 0.5.3 Determination of lead and copper content Flame atomic absorption spectrophotometry (arbitration method) 5.3.1 In a nitric acid medium, collect spectrophotometers at wavelengths of 283.2 nm and 228.4 nm respectively, increase the air temperature, and use the standard curve to determine the lead and copper content. 5.3.2 Reagents and test equipment 5.3.2.1 Gas 5.3.2-2 Nitric acid solution: -11.5 5.3.2.3 Standard standard for lead: 133 mR/L
5.3.2.4 Standard rate of mercury: 0mg/1.
HG/2844 was authorized to prepare 1 standard source. The standard source was used for the standard. The water was used accurately in Section 10. 5.3.3 Instruments and equipment
5.3.3.1 Absorption spectrophotometer.
5.3.3.2 Mercury and front pole lamp
5.3.4 Initial determination
5 3.4.1 Drawing of working curve
As shown in Figure 2, transfer the standard microfluid to a 1L bottle, add water to release the lead to the degree of absorption, and shake.
Table 2 The absorbance of the standard fluid and the corresponding standard liquid in the working curve. 5
g quality np
Note: The preparation of the international Xi elastic fluid can refer to the amount of lead contained in the product. The absorption rate is appropriately adjusted. s. n
Based on the properties of the element to be measured, the optical potential bandwidth, the ratio of the lamp, the high interest rate of the burner, and the air-flow rate are measured on the test line. Then, at the wavelength of 293.3, adjust the absorbance of each standard microfluid with water to zero and determine the absorbance. Take the mass of each standard solution as the reference value. The corresponding absorbance is the value of the curve. 5.3.4.2 Sample determination
Take 5-25% zinc sulfate sample to <00) . Add 5ml of water, add 5ml of nitric acid, and transfer to 1ml mother bottle after decomposition. Drain with water to measure, evenly spread, and discard the first few liters of the sample for determination of lead content. Determine the absorbance of the sample at the same time as the standard solution, and find the corresponding absorbance on the curve. If necessary, dilute with water for a certain amount and continue
At the same time, start the empty test from the preparation of the sample. 5.3.4.3 Analysis results* Expressed as fractions of lead (Ph) (X3) (X3) (X1) (X3 ... ck5
Details
5.3.5 Correction
5.3.5.1 Working curve setting
.0c5~-.e1
> 0. 010 -- 0, 020
According to Table 4, take 100L of standard liquid in 7 pots, add 5m1. acid, grind to dilute, spread evenly, the standard liquid volume and corresponding mass of standard liquid in Table 4 working curve are drawn, 1
HB
juice, standard setting, can be determined according to the sample energy content and other parameters of the instrument. According to the properties of the test element, the light bandwidth, lamp current, burner height, air The working conditions are selected, and then the wavelength is 228.8, and the absorbance of each standard sieve solution is measured. The mass of each standard solution is used as the coordinate, and the corresponding absorbance is used as the new coordinate to make a grade curve. 5.3.5.2 Sample determination
Take 1.5 g of cadmium sulfate sample (accurate to 0.001g), add 30 mL of water, and draw ml of membrane solution. After decomposition, transfer it into a 1CC bottle and dilute it to the scale with oil and water, filter it, and use it for determination of content. Measure the absorbance of the test solution in the presence of a standard solution and find the amount of absorption on the working curve. If necessary, measure again after a certain amount of water is released. Simultaneously, start the test from the beginning. 5.3.5.3 Analysis results: Expression of the absorbance of the test solution expressed as mass fraction (d) (X,> calculated according to formula (1), xn×100
Wu: 1
According to the absorbance of the test solution, find the amount of absorption from the end of the test solution, and according to the measured air Verify the absorbance obtained from the working curve: the screening result is reliable.
Take the half-mean of the parallel determination results as the determination result. 5.3.5.4
The absolute value of the parallel determination results shall meet the requirements of Table 5. The table contains the allowable absolute difference of the determination results. %
First, the allowable absolute difference, 5
5.1 Determination of lead and thionium content
5.4.1 Method source
>6.C3--5.012
>(0. (tU 0. u2U
) In the potassium fluoride-salt filter, with animal gelatin or dead olefins to inhibit the enzyme, oxygen is passed through, and within the voltage range of 0.20.5V, a good polarographic waveform is continuously drawn. 5.4.2 Reagents and materials
This method uses deionized water of appropriate purity. 5.4.2.1 Hydrogen in a cylinder.
5.4.2.2 Acid solution: 111.
5.4.2.3 Acid solution, 1+11.
5.4.2.4 Potassium oxide solution: 75$/1.
5.42.5 Protective film solution: 20g/L
5.4.2.6 Animal glue or polyvinyl alcohol (PVA) solution: 5g/L, animal glue solution should be prepared before use. 5.4.2.7 Standard solution: 100mg/L.
5.4.2.8 Standard solution of saw: 100mg.
5.4.3 Instruments and equipment
Anode instrument:
The anode of the electrolytic cell can be made of calomel and silver-silver electrode: collect a silver wire of about 20cm in diameter into a spiral shape, clean it with nitric acid, and then rinse it with distilled water, and carry out electrolysis in the electrolyte, with the silver wire as the anode, a pin or an incomplete rod as the cathode, and a DC source of 1.3V. Current: Only the electric efficiency is measured until the surface is broken. A small section of the induction tube (10cm5mm) is used at one end to support the latex resin, but the resin should not be raised when burning. In a glass tube, potassium chloride is dissolved. The surface of the solution is chlorinated. The solution is also chlorinated. The solution is also chlorinated. The solution is chlorinated. The solution is chlorinated. The solution is chlorinated. The solution is chlorinated. The solution is chlorinated. The solution is chlorinated. The solution is chlorinated. The solution is chlorinated.Slightly boil water and 1 mL of water, store on high heat until the gold is completely dissolved. Cool and transfer the solution to a 50 mL bottle, add 5 L of ascorbic acid solution, 1 mL of potassium hydroxide solution and 0.5 mL of animal cavity fluid (enol solution). Dilute with water to the mark, add 5 HG 32772000
Pour part of the liquid into the electrolyte and expose it to the atmosphere for 5~10min. Select an appropriate quenching temperature and apply an internal pressure of 0.3~-0.8V to carry out the Mannheim determination of the solution.
5.4.4.2 Determination of standard solution
Separately weigh about 1 μg (accurate to C.1) of zinc sulfate test product into 10 ml of calcined water and add a little water and 3 ml of 1.5% chlorinated sodium sulfate. Heat on an electric furnace until it is completely dissolved. Transfer the sieved liquid into a mother bottle and accurately add the standard solution and the standard solution with the contents of lead and potassium in the sample. Add 5 ml of ascorbic acid solution and 5 ml of sodium chloride solution in turn. Stir and 1mL animal glue drop me (form u.5ml. ene alcohol solution), water ene select Liu degree, probe spoon. Double according to 5.4.4.1 required steps to complete the source determination. 5.4.5 Analysis station results
with the quality of the user to show the language (Pb) or pyrolysis (Pb) content (X, according to the formula (5) x, =
two (h,)
where
test solution wave mn
standard comparison minus dial height.mm
standard comparison solution add lead (Pb) quality + ruler) - sample quality B.
four parallel determination results are the arithmetic average of the results of the determination. 5.4. 6 Allowable absolute value of the traceability result: lead, to 5.3.4.4: 5.3.5.5 Determination of arsenic content Diethyl dihydrogen arsenic spectrophotometry (arbitration method) 5. ... m,
5.5.2.2 Diethyl monoxide (C,IIs), NCS;AL Ag(DDTC)J-pyridine solution: 5g/L: 5.5.2.3 Acid solution: c1/2HS),) = 15mol/L, take 420ral. High-grade vegetable, slowly pour into about 580mL water, cool. Mix, 5.5.2.4 Acetic acid saturated solution: 250yuan/1..5.5.2.5 Acetic acid according to the flower.
5.5.2.6 Potassium borate solution, 150g/L.
Float for 15s Potassium borate in water. Add water to 1uumt, evenly 5.5.2.7 Chemical industry salt waist float: 40R/T.5.5.2.8 Float: 130m/1. 5.5.2.9 Standard extract: 2.30g/1.
Pick up 25ml of the standard solution (5.5.2.8) into a 1L volumetric flask, dilute to scale with water, and spread evenly. Preparation: 5.5.3 Receiver, equipment
5.5.3.1 Spectrometer and 1cm absorption cell.
5.5.3.2 Surface of hydrogen generator (as shown in Figure 2) 1IG32772000
European absorption drink
Explosion link
V= 100ngt,
Ethylene oxide
Quickly generate pressure
2Hydrogen oxidizer (unit: m)
e, conical flask, with 100ml, used for hydrogen oxidization, b. Connector, before use, fill with lead acetate cotton e. 15 small bulbs to absorb solution, total thickness of about 250mm, total volume 14mL, note, all the reduced substances in the extraction instrument need to be washed with fuel acid-heavy potassium filter, and then thoroughly washed with water and refined, 5.5.4 determination|| 5.5.4.1 Before the working curve is given, as shown in Table 6, aspirate the standard liquid (5.5.2.) into a cone. The standard liquid and the standard liquid in the working curve in Table 6 are aspirated according to the volume. Add 1 ml to each cone. Add 2 ml of sulfuric acid solution and a certain amount of base water to 10 ml. Mix the sulphuric acid solution and 2 ml of chlorinated melt and place for 15 minutes. Place a small amount of chlorine in the connecting tube. In the absorbent, transfer 1 ml A (DDTC)-pyrrolidone to the absorbent, connect the instrument as shown in Figure 2: weigh the granules and add them to the detailed bottle, connect the instrument as quickly as possible, and let the reaction proceed for about 45 minutes. Remove the absorber, fully filter the effective red silver, and use 1 c absorption cell at a wavelength of 540 nm. Take the solution with zero corrosion content as the reference solution as the quarterly quotient, adjust the spectrophotometer until the absorbance of the reference solution is zero, and then perform absorbance determination.
Dissolved wavelength set about 2 , the determination is carried out in this period, with the amount of gold () as the horizontal standard, and the corresponding film absorbance as the natural half-scale Tu
standard to prepare the working curve:
HG:3277—2000
Every month, the newly prepared A (DDIX)-pyridine should be used, and each time a new batch of zinc particles is used, a new natural working curve should be prepared. 5.5.4.2 Sample measurement
Place the sample in a light test bottle (accurate to ) on an energy-shaped bottle. The sample contains 20 mL of water and defrost to 301 mL. Add 1) mL of mineral oil, 2 mL of potassium hydroxide solution and 2 mL of sodium phosphate in sequence. Boil the mixture and add 1>trin. According to the provisions of 5.5.1.1, the test results are as follows. 5.5.5 The analysis of the short report is based on the test results. The iodine content (As) expressed as a percentage of the amount is calculated according to formula 6: X.
In the formula, the amount of nutrients in the food and the liquid of the worker is full! Test quality base number:
National two-way light formulation conclusion The arithmetic value of the result is taken as the determination result. The absolute difference between two parallel determinations of oxygen content is not more than 12%. 5.6 Determination of content by the method 5.6.1 Summary of the method In a phase medium, the chemical reagent is used to react with the test paper based on the chemical reaction of hydrogen peroxide and the reaction of the test paper with different effect standards and standard liquids to obtain a series of standard color scale comparisons. 5.6.2 Reagents and materials 5.6.2.1 0.5-1 mm.
5.6.2.2 Chemical test,
5.62.3 Hydroxy acid solution: ?2H03/..
Measure 42ml of extremely pure chlorinated acid, inject into 583ml of water, cool and mix well, 5.6.2.4 Acetyl alcohol solution: 200g/L. 5.6.2.52 Alkyl lead dilution ratio
5.6.2.6 Potassium hydroxide solution: 15Vg/L
Dissolve 1ml of the solution in water and dilute with water
5.6.2. Chemical industry solution: 400g/.
5.6.2.8 Standard solution, 100mg/..
5.6.2.9 Standard solution: 0.1g.
Take 23T. The liquid is <.2.A) in ten quantities, two light water, and then spoon. Preparation for use: 5.6.3 Only equipment, transportation equipment
IIG3277
Winning width
Main 3 upper tube 1
To be determined (unit m)
5.6.3.1 Volume, capacity plate 125mi. Use Ding Zhong oxygen generation 5.63.2 Glass height: length 18m, upper diameter center: mm, the technical end of the tube has a diameter of about 2nm, before use, install the person B afraid of brown high mm.bZxz.net
5.6.3.3 Nuclear rate snow school tube mouth, surface polished, the following has a about: regret with the same glass increase. 5.G3.4 Drum finger, grind half, center with a diameter of 6.5mm, with a moon-shaped tip below, when single, use chemical test paper to fix the tube mouth on the glass, etc. 5.6.4 Fixation
5.6.4.1 Preparation of standard steps
Multiple cores are taken, 1.0mL, 2.0I4.0mL, 6.0ml. and 8.0ml. Standard depth (5.G.2.9) is placed at 5 Add 2M potassium iodide solution and 2M iodine chloride solution to each bottle, place a small amount of 15% sodium iodide solution in a tube, and let the absorbent react for 3 minutes. Then, add the test paper 5.6.4.2 to obtain a certain amount of the sample. The sample contains no more than 23g of mother. Add 1 (m.Add enough water to make the volume about 40ml. Add 2mL potassium iodide and 2mL stannous chloride, mix and place in a mixture for 15min. 5. Complete the test as specified in 4.1. Take the test paper and compare it with the standard color scale. 5.6.5 Analyze the results of the test. The content of A) expressed as a percentage of denier is calculated according to the formula: X =
Formula: m:
Compared with the standard color scale, the test amount (7)
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