Some standard content:
Record number: 2764-1999
HG/T3582-1999
This standard is formulated in accordance with the requirements of manufacturers and users and with reference to enterprise standards. Compared with domestic enterprise standards: 1 This standard is divided into two categories: liquid and solid. Solids are divided into two grades: first-class products and qualified products; liquids are divided into grades. 2 The index items set by each enterprise standard are different. This standard uniformly sets seven indicators according to user requirements; zinc nitrate [Zn (N () : 6H.OI content, free acid (in terms of HN () :) content, heavy metals (in terms of Pb), iron (Fe), sulfate (in terms of SO), chloride (in terms of CI), water insoluble content.
3 The test method is greatly improved compared with the enterprise standard, and all items are determined by classic test methods. Appendix A of this standard is the appendix of the standard. 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 inorganic salt product standardization technology unit of the Ministry of Chemical Industry. The drafting units of this standard are: Tianjin Chemical Research Institute of the Ministry of Chemical Industry and Hunan Chemical Reagent Factory. The main drafters of this standard are: Liu Shuying, Yin Zhaowu and Lin Wenxin. This standard is entrusted to the technical unit responsible for the standardization of inorganic salt products of the Ministry of Chemical Industry for interpretation. 1056
1 Scope
Chemical Industry Standard of the People's Republic of China
Industrial zinc nitrate
Zine nitrate for industrial useHG/T 3582--1999
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation and storage of industrial zinc nitrate. This standard applies to industrial zinc nitrate. This product is mainly used as an anti-rust phosphating agent for metal surfaces, and is also used as a fabric mordant and a preservative for synthetic substances.
Molecular formula: Zn(NO,)·6H2O
Relative molecular mass: 297.49 (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. GB190—1990 Labeling of dangerous goods for packaging
—1990 Pictorial marking of packaging, storage and transportation
GB 191-
GB/T 601—1988
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents Preparation of standard solutions for determination of impurities of chemical reagents (neqISO6353-1:1982)GB/T602--1988
GB/T 603-- 19881
Preparation of preparations and products used in chemical reagent test methods (neqISO6353-1:1982)GB/T 610. 1—1988
General method for determination of arsenic in chemical reagents (arsenic spot method)GB/T1250—1989
Expression and determination method of limit valuesGB/T 6678---1986
General rules for sampling of chemical products
GB/T6680—1980General rules for sampling of liquid chemical productsGB/T 6682-19922
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987)GB/T 8946 ---1988
GB/T 8947-1988
3 Product classification
Plastic woven bags
Composite plastic woven bags
Industrial zinc nitrate is divided into two categories: liquid and solid. 4 Requirements
4.1 Appearance: The solid is colorless or white block or granular crystals. The liquid is a slightly yellow transparent liquid. 4.2 Industrial zinc nitrate should meet the requirements of Table 1. Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999 and implemented on April 1, 2000
Zinc nitrate [Zn(NO,): 6H2O] content
Free acid (as HNO,) content
Iron (Fe) content
Heavy metal (as Pb) content
Sulfate (as SO) content
Water-insoluble matter content
Chloride (as CI) content
5 Test method
HG/T 3582—1999
Table 1 Requirements
Qualified products
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB/T6682-1992.
The standard titration solution, impurity standard solution, preparation and product used in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
5.1 Determination of zinc nitrate content
5.1.1 Summary of the method
Heavy metal ions such as iron and lead are shielded with ascorbic acid and potassium sodium tartrate. The zinc in the test solution is complexed with disodium ethylenediaminetetraacetate (EDTA). The content of zinc nitrate is calculated based on the amount of EDTA consumed. 5.1.2 Reagents and materials
5.1.2.1 Ascorbic acid solution: 20 g/L;
2 Potassium sodium tartrate solution: 200 g/L;
5. 1. 2. 2
Acetic acid-sodium acetate buffer solution: pH 6;
5.1.2.4 Disodium ethylenediaminetetraacetic acid standard titration solution (EDTA): c(EDTA) is approximately 0.05 mol/L; Xylenol orange indicator solution: 2 g/L (store for 1 to 2 weeks). 5. 1.2.5
5.1.3 Analysis steps
Weigh 0.4g (0.5g for liquid) sample (accurate to 0.0002g), place it in a 250mL conical flask, add 75mL water to dissolve, add 10ml ascorbic acid solution and 5mL potassium sodium tartrate solution, add 10mL acetic acid-sodium acetate buffer solution, add 2 drops of xylenol orange indicator solution, and titrate with EDTA standard titration solution until the solution changes from purple-red to bright yellow, which is the end point. 5.1.4 Expression of analysis results
The content of zinc nitrate [Zn(NO,)2·6H,O] expressed as mass fraction (X,) is calculated according to formula (1): Xi = Ve X0.2975 × 100 = 29.75 ×Vem
Wherein: V--the volume of EDTA standard titration solution consumed by the titration test solution, mL; ---the actual concentration of EDTA standard titration solution, mol/L; the mass of the sample, g;
.....( 1)
where ++ying yiying
0.2975—…is the mass of zinc nitrate hexahydrate expressed in grams equivalent to 1.00mL FDTA standard titration solution [c(EDTA)=1.000mol/L].
5.1.5 Allowable difference
HG/T 3582—1999
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 5.2 Determination of free acid content
5.2.1 Summary of method
Use methyl orange as the indicator solution and titrate with sodium hydroxide standard titration solution to determine the free acid content. 5.2.2 Reagents and materials
5.2.2.1 Carbon dioxide-free water;
5.2.2.2 Standard sodium hydroxide titration solution: c(NaOH) is about 0.02 mol/L; 5.2.2.3 Methyl orange indicator solution: 10 g/L. 5.2.3 Analysis steps
Weigh about 5g of sample (accurate to 0.01g), place in a 250mL conical flask, add 50mL of carbon dioxide-free water to dissolve the sample, add 2 drops of methyl orange indicator solution, and titrate with sodium hydroxide standard titration solution until the solution changes from red to yellow. 5.2.4 Expression of analysis results
The free acid content (in terms of HNO3) expressed as mass fraction (X2) is calculated according to formula (2): X Ve × 0. 063 01 × 100 m
Wherein: V-
6. 301 X Vc
The volume of NaOH standard titration solution consumed by the titration test solution, mL; the actual concentration of NaOH standard titration solution, mol/L; m-the mass of the sample, g;
0.06301-——the mass of nitric acid expressed in grams equivalent to 1.00ml NaOH standard titration solution Lc (NaOH) = 1.000mol/L.
5.2.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.003%. 5.3 Determination of iron content
5.3.1 Method Summary
In an acidic medium, add thiocyanate to make iron into a red complex of thiocyanate iron, extract with n-butanol, and compare with the standard colorimetric solution.
5.3.2 Reagents and Materials
5.3.2.1 n-butanol;
5.3.2.2 Hydrochloric acid solution: 1+1;
5.3.2.3 Ammonium thiocyanate solution: 250g/L; 5.3.2.4 Iron standard solution: 1mL solution contains 0.1mgFe. 5.3.3 Analysis Steps
Weigh (5.00±0.01)g of sample, place in a 100mL volumetric flask, add water to dissolve, dilute with water to the mark, and shake. This is solution A. Reserve for the determination of heavy metals. wwW.bzxz.Net
Use a pipette to transfer 10ml of solution A into a 50ml colorimetric tube, dilute to 25ml with water, add 1ml hydrochloric acid solution, 2ml ammonium thiocyanate solution and 5ml n-butanol, shake vigorously, the red color of the alcohol layer should not be darker than the standard colorimetric solution. Preparation of standard colorimetric solution: Take a certain volume of iron standard solution and treat it in the same way as the test solution according to the following regulations. Solid: 0.5ml for -standard product, 1.0ml for qualified product; liquid: 0.25ml. 5.4 Determination of heavy metal content
Safety tips: The sodium cyanide (or potassium cyanide) used in this test is a highly toxic drug. Be careful when using it, prepare safety equipment, and avoid contact or inhalation. See Appendix A for the treatment of cyanide-containing waste liquid. 5.4.1 Method Summary
In alkaline medium, sodium cyanide (or potassium cyanide) is used to mask interfering ions, and sodium sulfide reacts with heavy metal ions such as lead to generate brown-yellow color, 1059
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and standard colorimetric solution is used to determine the content of heavy metals in the sample. 5.4.2 Reagents and Materials
5.4.2.1 Ammonia solution: 2+-3;
5.4.2.2 Sodium cyanide (or potassium cyanide) solution: 100g/L: 5.4.2.3 Sodium sulfide solution: 100/1 (freshly prepared); 5.4.2.4 Lead standard solution: 1ml. The solution contains 0.1mgPb. 5.4.3 Analysis steps
Use a pipette to transfer 1.0 ml of solution A (5.3.3) into a 50 ml colorimetric tube, add water to dilute to 25 ml, adjust the pH to about 8.5 with ammonia solution (check with precision pH test paper), add 10 ml of sodium cyanide (or potassium cyanide) solution, and shake to hook. Add 1 ml of newly prepared sodium sulfide solution, dilute to the mark with water, and shake to hook. Let stand for 10 min, the color should not be darker than the standard colorimetric solution. Preparation of standard colorimetric solution:
According to the following rules, transfer a certain volume of lead standard solution into a 50 ml colorimetric tube, and treat it in the same way as the test solution. Solid: 0.25 ml for first-class products, 1.5 ml for qualified products; liquid: 1.25 ml. 5.5 Determination of sulfate content
5.5.1 Method summary
In hydrochloric acid medium, sulfate radicals and barium ions generate white fine barium sulfate precipitates, which are turbidometrically compared with standard turbidimetric solutions. 5.5.2 Reagents and materials
5.5.2.1 Hydrochloric acid solution: 1+1;
5.5.2.2 Hydrochloric acid solution: 1+2;
5.5.2.3 Chlorinated sodium solution: 250 g/L;
5.5.2.4 Sulfate standard solution: 1 mL of solution contains 0.1 mg S). 5.5.3 Analysis steps
Weigh (1.00±0.01)g of sample, place in an evaporating dish, add 2mL of hydrochloric acid solution (5.5.2.1) and evaporate to dryness in a water bath. After cooling, dissolve the residue with 25ml of water and transfer to a 50mL colorimetric tube, add 1ml of hydrochloric acid solution (5.5.2.2), add 3mL of barium chloride solution, dilute to scale, shake well, keep warm at 30℃～35℃ for 10min, and compare its turbidity with the sulfate standard turbidity solution series. Preparation of sulfate standard turbidity solution: Transfer an appropriate amount of sulfate standard solution into a 50ml colorimetric tube, prepare a standard series and treat it in the same way as the test solution.
5.5.4 Expression of analysis results
The sulfate content (in terms of SO) expressed as mass fraction (X:) is calculated according to formula (3): X:=×0. 0001×100:
Wherein: V—the amount of sulfate standard solution, ml; the mass of the test material, g;
0.0001:—the mass of sulfate ions in 1.00 ml sulfate standard solution, g. 5.6 Determination of water-insoluble matter content
5.6.1 Instruments and equipment
5.6.1.1 Glass crucible: pore size 5 μm~15 μm; 5.6.1.2 Electric oven: temperature can be controlled at 105℃~110℃, 5.6.2 Analysis steps
(3)
Weigh about 20g sample (accurate to 0.0002g), place it in a 250ml beaker, add 100mL water until the sample is dissolved, heat and boil for 10min, filter while hot using a glass crucible that has been dried at 105℃~110℃ to constant weight, wash with hot water 3~4 times, 30mL of water each time, place the glass crucible in an oven at 105℃~110℃ to dry to constant weight, take out and place in a desiccator to cool before weighing. 5.6.3 Expression of analysis results
HG/T 3582—1999
The water-insoluble content (X.) expressed as mass fraction is calculated according to formula (4): X
Wherein: mi
Mass of the residue after drying, g;
Mass of the sample, g.
5.6.4 Allowable difference
ml×100
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.02%. 5.7 Determination of chloride content
5.7.1 Summary of method
In nitric acid medium, the chloride ions in the test solution react with silver nitrate to generate silver chloride, which is determined by visual turbidimetry. 5.7.2 Reagents and materials
5.7.2.1 Nitric acid solution: 1+2;
5.7.2.2 Silver nitrate solution: 17g/L.;
5.7.2.3 Chloride standard solution: 1ml. The solution contains 0.1mgCl. 5.7.3 Analysis steps
(4)
Weigh (1.00±0.01)g of sample, place it in a 50mL colorimetric tube, add 25mL water to dissolve, add 2mL nitric acid solution and 1mL silver nitrate solution, shake well, let it stand for 10min, and compare it with the chloride standard turbidimetric solution series. Preparation of chloride standard turbidimetric solution:
Pipette an appropriate amount of chloride standard solution into a 50mL colorimetric tube to make a standard series, and treat it in the same way as the test solution. 5.7.4 Expression of analysis results
The chloride (Cl) content (X,) expressed as mass fraction is calculated according to formula (5): X: V×0.000 1×100 - 0. 01×Vm
Wherein: V——the amount of chloride standard solution, mL; m the mass of the test material, g;
0.0001---1.00mL the mass of chloride ions in the chloride standard solution, g. 6 Inspection rules
6.1 This standard adopts type inspection and routine inspection. All seven index items specified in the requirements are type test items, among which zinc nitrate content, free acid content, iron content, and heavy metal content are routine test items and should be tested batch by batch. Under normal production conditions, type test shall be carried out at least once every three months.
6.2 Each batch of products shall not exceed 20t.
6.3 Determine the number of sampling units in accordance with the provisions of 6.6 of GB/T6678-1986. Solid: Each iron barrel or plastic woven bag is a packaging unit. When sampling, insert the sampler obliquely to 3/4 of the depth of the material layer to take samples. From each selected packaging unit, take out no less than 50g of sample, mix the sampled sample and reduce it to about 500g by quartering method, and immediately put it into two clean and dry wide-mouth bottles with ground-mouth stoppers and seal them. Paste labels on the bottles, indicating the manufacturer's name, product name, category, grade, batch number, sampling date and name of the sampler. One bottle is used as a laboratory sample, and the other bottle is kept for three months for reference. For liquid products, use a glass sampling tube to vertically insert it into the 3/4 of the packaging barrel for sampling. The total sample volume is not less than 500mL and is stored in a ground-mouth glass bottle.
6.4 Industrial zinc nitrate should be inspected by the quality supervision and inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer should ensure that each batch of products shipped out of the factory meets the requirements of this standard.
If any index of the inspection result does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-inspection. If even one index of the re-inspection result does not meet the requirements of this standard, the entire batch of products shall be unqualified. 1061
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6.5 According to 5.2. The rounded value comparison method specified in the regulations shall be used to determine whether the test results comply with the standard. 7. Marking, packaging, transportation and storage
7.1 The packaging bag of industrial zinc nitrate should be firmly and clearly marked, including the manufacturer's name, address, product name, trademark, category, grade, net content, batch number or production date and the number of this standard, as well as the "oxidant" mark and "toxic" mark specified in GB190, and the "wet-afraid" mark specified in GB191.
7.2 Each batch of industrial zinc nitrate leaving the factory should be accompanied by a quality certificate. The content includes the manufacturer's name, address, product name, trademark, category, grade, net content, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 7.3 Packaging of industrial zinc nitrate: Solids can be packaged in iron drums lined with two layers of plastic bags or polypropylene woven bags. Woven bag packaging: the inner packaging is a polyethylene plastic film bag with a thickness of not less than 0.08mm, and the outer packaging is a polypropylene woven bag. Its performance and inspection methods should comply with the relevant provisions of GB/T8946B. The net content of each bag of this product is 25kg and 40kg. Iron barrel packaging: the inner packaging is a polyethylene plastic film bag with a thickness of not less than 0.08mm, and the outer packaging is a special, sealed fully open iron barrel with a wall thickness of 0.5mm~0.75mm. The net content of each barrel is 50kg. Liquids are packaged in plastic barrels with a net content of 20kg and 25kg per barrel. Woven bag packaging: When packaging, industrial zinc nitrate is placed in a polypropylene woven bag lined with two layers of polyethylene plastic film bags, and the remaining air in the bag is discharged. The two layers of inner bag mouths are tied four times with a rope and tied tightly. The outer bag is sewn with a bag sewing machine at a distance of not less than 15mm from the upper end of the bag. The stitches are neat and the stitches are evenly hooked. There are no leaks or skipped stitches. When using iron drum packaging, put industrial zinc nitrate into a special, sealed, fully open iron drum lined with two layers of polyethylene plastic film bags, exhaust the remaining gas in the bag, tie the two layers of inner bag mouth with rope four times, cover the drum lid and seal it. 7.4 Industrial zinc nitrate should be covered during transportation to prevent sun exposure, rain, and packaging damage. It should not be transported with organic matter, reducing agents, and acids to prevent explosion.
7.5 Industrial zinc nitrate should be stored in a cool, dry and ventilated warehouse to prevent sun exposure, moisture, and packaging damage. It should not be stored with organic matter, reducing agents, and acids, and should be kept away from fire and heat sources to prevent explosion. 1062
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Appendix A
(Appendix to the standard)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the cyanide waste liquid should be post-treated after daily analysis before it can be discharged. A1 Method Summary
Under alkaline conditions, divalent iron and cyanide ions form stable complex ions. A2
Analysis Steps
Collect the waste liquid in a 500mL beaker, add 50mL of 200g/L ferrous sulfate solution, stir, and discharge after sufficient reaction. The above-mentioned reagents are all industrial grade.
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