Some standard content:
Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG 2565-94
This standard specifies the technical requirements, test methods, inspection rules, as well as marking, packaging, transportation and storage of industrial potassium aluminum sulfate. This standard applies to industrial potassium aluminum sulfate processed from natural alum stone. It is mainly used in water purification, paper sizing, coating printing and dyeing, aquatic product pickling, pharmaceuticals, leather making, rubber and colored glass industries. Fraction: AIK(SO4)·12H,O or Al2(SO)3·K,SO·24H0Relative molecular mass: 474.39 or 948.78 (according to the international relative atomic mass in 1989)2Reference standards
GB 191
Pictorial symbols for packaging, storage and transportation
GB/T 601
GB/T 602
GB/T 603
GB 1250
Chemical reagents
Preparation of standard solutions for titration analysis (volume analysis)Chemical reagents
Preparation of standard solutions for impurity determination
Preparation of preparations and products used in chemical reagent test methodsExpression and determination methods of limit valuesGB/T 3049
GB/T 6678
GB/T 6682
GB8450
GB 8451
GB 8946
GB 8947
3 Technical requirements
General method for determination of iron content in chemical products O-phenanthroline spectrophotometric method General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories Determination of arsenic in food additives
Limit test method for heavy metals in food additives Plastic woven bags
Composite plastic woven bags
3.1 Appearance: colorless, transparent, translucent block, granular or crystalline powder. 3.2
T. Potassium aluminum sulfate should meet the requirements of the following table:% m/m
Potassium aluminum sulfate (AIK(SO,)2·12H,O) content (dry basis)Iron (Fe) content (dry basis)
Heavy metal (Pb) content
Arsenic (As) content
Water insoluble matter content
Approved by the Ministry of Chemical Industry of the People's Republic of China on February 9, 1994532
Superior product
First-class product
Qualified product
Implemented on July 1, 1994
4 Test method
HG 2565-94
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and grade 3 water specified in GB/T6682. The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603. 4.1 Determination of Potassium Aluminum Sulfate Content
4.1.1 Method Summary
In an acidic medium, EIDTA forms a complex with aluminum, and the EITA is back-titrated with lead nitrate. Thus, the content of aluminum sulfate can be determined. 4.1.2 Reagents and materials
4.1.2.1 Hydrochloric acid (GB/T622) solution: 1+4; Ammonia (GB/T631) solution: 1+1;
4.1.2.3 Acetic acid-sodium acetate buffer solution: pH=6;4.1.2.4 Disodium ethylenediaminetetraacetic acid (EDTA) (GB/T1401) standard titration solution: c(EDTA) is about 0.05 mol/L;4.1.2.5 Lead nitrate (HG/T3-1070) standard titration solution: cLPb(NO;)2 is about 0.05 mol/l.;4.1.2.6
I. Cresol orange indicator solution: 2 g/L;
Congo red test paper.
4.1.3 Analysis steps
Weigh 5g of the sample (accurate to 0.0002g) ground and dried according to 4.6.3, place it in a 150mL beaker, add 80ml of water, and heat to dissolve. After cooling, transfer it to a 250mL volumetric flask, add 10 drops of hydrochloric acid solution, dilute with water to the scale, and shake well (if turbid, filter and discard the initial filtrate). This is solution A.
Use a pipette to transfer 50mL of solution A and place it in a 250mL conical flask. Use a pipette to transfer 50ml of ethylenediaminetetraacetic acid = sodium standard titration solution, add a small piece of Congo red test paper, and then use ammonia solution to adjust the test paper to purple red (pH5-6), add 15ml of acetic acid-sodium acetate buffer solution, boil for 3min, cool, add 3-4 drops of xylenol orange indicator solution, and titrate with lead nitrate standard titration solution until the orange-yellow end point. Perform a blank test at the same time.
4.1.4 Expression of analytical results
The content X of potassium aluminum sulfate (AIK(SO)·12H,O) expressed as mass percentage is calculated according to formula (1): (V.-V) cX0.4744×100-X, X8.49X, =
m×250
= 237. 2c(V.-V)
—8.49X2bzxZ.net
Wu Zhong: c—actual concentration of standard lead nitrate titration solution, mol/L; V—volume of standard lead nitrate titration solution consumed in titrating blank, mL; V---volume of standard lead nitrate titration solution consumed in titrating test solution, ml. X.-—percentage of iron determined according to 4.2, %; mass of sample, g;
0).4744——mass of potassium aluminum sulfate expressed in grams equivalent to 1.00mL standard lead nitrate titration solution (cCPb (NO.),]=1.000mol/L);
coefficient for converting iron into potassium aluminum sulfate.
4.1.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.2%. 4.2 Determination of iron content
4.2.1 Summary of method
Same as Article 2 of GB/T3049.
4.2.2 Reagents and materials
Same as Article 3 of GB/T3049.
4.2.3 Instruments and equipment
Spectrophotometer: with 3cm absorption cell 4.2.4 Drawing of working curve
HG 2565—94
According to Article 5.3 of GB/T3049, use 3cm absorption cell and corresponding amount of iron standard solution to draw working curve. 4.2.5 Analysis steps
Use a pipette to transfer 50mL (superior and first-class products) or 10mL (qualified products) of solution A (4.1.3) into a 100mL volumetric flask, then take 50mL of water into another 100mL volumetric flask, add water to about 60mL, adjust the pH to about 2 with hydrochloric acid solution, and check the pH with precision pH test paper. The following operations are carried out according to Article 5.4 of GB/T3049 from "adding 2.5mL of ascorbic acid solution to measuring the absorbance of the solution".
4.2.6 Expression of analysis results
The iron content X expressed as mass percentage is calculated according to formula (2): X2
m-×100
m×250
25(m-mo)
Where: m,——according to the measured The mass of iron found from the working curve according to the absorbance of the test solution, mg; - the mass of iron found from the working curve according to the measured absorbance of the blank test solution, mg; mo
V-—the volume of solution A (4.1.3) transferred, mL, m
mass of the sample, g.
4.2.7 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result, and the absolute difference of the parallel determination results Not more than 0.003%. 4.3 Determination of heavy metal content
4.3.1 Method summary
Same as Article 2 of GB8451.
4.3.2 Reagents and materials
4.3.2.1 Hydroxylamine hydrochloride (GB/T6685); 4.3.2.2 Acetic acid (GB/T676) solution: 300g/L; 4.3.2.3 Saturated hydrogen sulfide solution, prepared immediately before use; 4.3.2 .4 Hydrochloric acid (GB/T622) solution: 1+3; 4.3.2.5 Lead standard solution: 1mL solution contains 0.01mgPb; (2)
Preparation: Use a pipette to transfer 10mL of the lead standard solution prepared according to GB/T602 into a 100mL volumetric flask, dilute with water to the mark, and shake well. This solution is prepared when used. 4.3.3 Analysis steps
Weigh 5.0g of the ground sample (accurate to 0.01g), placed in a 100mL beaker, dissolved in water, transferred to a 100mL volumetric flask, diluted with water to the mark, and shaken. Dry filter, use a pipette to transfer 20mL of filtrate, placed in a 50mL colorimetric tube, add water to 25mL, add 5 drops of hydrochloric acid solution, 0.1g hydroxylamine hydrochloride, 0.5mL acetic acid solution, 10mL saturated hydrogen sulfide solution, dilute with water to the mark, and shake well. Place in a dark place for 10 minutes, and the color should not be darker than the standard colorimetric solution. The standard colorimetric solution is to transfer 2mL (superior product, first-class product) or 5mL (qualified product) of lead standard solution, placed in a 50ml colorimetric tube, 534
HG 2565—94
Start by adding water to 25ml…”, and treat it in the same way as the test solution. 4.4 Determination of arsenic content
4.4.1 Summary of the method
Same as Article 2.1 of GB8450.
4.4.2 Reagents and materials
Arsenic-free zinc (GB/T2304);
Hydrochloric acid (GB/T622);
Potassium iodide (GB/T1 272) solution: 150g/L; 4.4.2.3
Stannoyl chloride (GB/T638) solution: 400g/L; Arsenic standard solution: 1mL solution contains 0.001mgAs; 4.4.2.5
Preparation: Use a pipette to transfer 10mL of the arsenic standard solution prepared according to GB/T602, place it in a 1000mL volumetric flask, dilute with water to the mark, and shake well. This solution is prepared when used. 4 .4.2.6 Lead acetate cotton;
Mercuric bromide test paper.
4.4.3 Instruments and equipment
Arsenic determination device: Same as Article 2.3 of GB8450.
4.4.4 Analysis steps
Weigh 1.00±0.01g of the ground sample, place it in an arsenic test bottle, add 25mL of water, 5mL of hydrochloric acid, 5mL of potassium iodide solution, and 5 drops of stannous chloride solution, and shake well. Place at room temperature 10min. Then add 3g of arsenic-free zinc, immediately plug the arsenic test tube pre-filled with lead acetate cotton and mercuric bromide test paper, and place it in the dark at 25-40℃ for 1h. Take out the mercuric bromide test paper, and the color of the arsenic spot should not be darker than the standard. The standard is to transfer 2mL (superior product), 5mL (first-class product), and 10mL (qualified product) of arsenic standard solution, place it in the arsenic test bottle, add water to 25mL, and start with adding 5mL of hydrochloric acid. ", and treat it in the same way as the sample at the same time. 4.5 Determination of water-insoluble matter content
4.5.1 Summary of the method
Dissolve the sample in water, filter it with a crucible filter, wash it with water, completely separate the main body of the sample from the filter residue, dry it, weigh it, and calculate the insoluble matter content.
4.5.2 Reagents and materials
Chloride (GB/T652) solution: 10g/L.
4.5.3 Instruments and equipment
Crock filter: pore size of filter plate 5μm~15um. 4.5.4 Analysis steps
Weigh about 20g of the ground sample (accurate to 0.01g), place it in a 250mL beaker, add 150mL boiling water, stir to dissolve, filter it through a crucible filter dried to constant weight at 105~110℃, wash the residue with boiling water until the filtrate does not contain SO-, (check with barium chloride solution). Dry it at 105~~110℃ to constant weight.
4.5.5 Expression of analysis results
Water-insoluble matter content X expressed as mass percentage: Calculate according to formula (3): X, - m2
ml×100
Where: m, the mass of the crucible filter, g; m2——the mass of the filter and water-insoluble matter after drying, g; m——the mass of the sample, g.
4.5.6 Allowable difference
(3)
HG 256594
Take the arithmetic mean of the parallel determination results as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.02%. 4.6 Determination of moisture
4.6.1 Summary of method
Dry the sample at a certain temperature and vacuum degree, and measure the reduced mass of the sample. 4.6.2 Instruments and equipment
4.6.2.1 Vacuum drying oven: can be controlled at 35±2°C, vacuum degree is 8093kPa (1mmHg=133.322Pa)4.6.2.2 Weighing bottle: $50mm×30mm; 4.6.2.3 Test sieve (GB6003) R40/3 series 200mmX50mm/355μm, 200mmX50mm/250μm. 4.6.3 Analysis steps
Grind the sample and sieve it with test sieves with apertures of 355μm and 250μm. Weigh about 5g of the sample with a particle size of 250~355um (accurate to 0.0002g) with a weighing bottle that has been pre-weighed at 35±2℃ and a vacuum degree of 80~93kPa. Place it in a vacuum drying oven and dry it for 1h at 35±2℃ and a vacuum degree of 80~93kPa. Weigh it. 4.6.4 Expression of analysis results
The moisture content X expressed as mass percentage is calculated according to formula (4): X.
Where: m—mass of the sample before drying, g; m\—mass of the sample after drying, g.
4.6.5 Tolerance
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.05%. 5 Inspection Inspection rules
(4)
5.1 Industrial potassium aluminum sulfate shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all industrial potassium aluminum sulfate products leaving the factory meet the requirements of this standard. Each batch of potassium aluminum sulfate products leaving the factory shall be accompanied by a quality certificate. The contents include: manufacturer's name, factory address, product name, grade, net weight, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 5.2 The user has the right to inspect and accept the industrial potassium aluminum sulfate products received in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 100t.
5.4 Determine the number of sampling units in accordance with Article 6.6 of GB/T6678. When sampling, use a sampling spoon to open the surface of the material and take out a representative sample of not less than 50g. Mix the sample thoroughly and use Use the quartering method to reduce the amount to about 500g, and pack it into two clean, dry wide-mouth bottles with ground stoppers and seal them. Paste labels on the bottles and indicate: manufacturer name, product name, grade, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other bottle is kept for three months for reference. 5.5 If any indicator in the inspection results does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging. If even one indicator in the inspection results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 5.7 Use the rounded value comparison method specified in (GB1250 to determine whether the inspection results meet the standards. 6 Marking, packaging, transportation, storage
6.1. The packaging bags of industrial potassium aluminum sulfate should have firm and clear markings, contents Including: manufacturer name, address, product name, trademark, grade, net weight, batch number or production date and this standard number, as well as the "wet-afraid" mark specified in GB191. 6.2 Packaging of industrial potassium aluminum sulfate: Block potassium aluminum sulfate adopts single-layer packaging, using type B composite plastic woven bags specified in GB8947, with specifications and dimensions: 900mm×550mm, and its performance and inspection methods should comply with the provisions of GB8947B type; granular and powdered potassium aluminum sulfate adopts double-film packaging. The inner packaging adopts polyethylene plastic film bags with specifications and dimensions: 1000mm×650mm, thickness of 0.06mm, and the outer packaging adopts plastic woven bags specified in GB8946, with specifications and dimensions: 900×550mm, and its performance and inspection methods should comply with the provisions of GB8946. When packaging industrial potassium aluminum sulfate, heat seal the inner bag, or tie the mouth and sew the plastic woven bag. Two stitches are made back and forth 15mm from the upper edge of the bag, with a stitch length of 6~~7mm, neat stitches, uniform stitch length, and no leaking or skipping stitches. The net weight of each bag of industrial potassium aluminum sulfate is 50kg. 6.3 Industrial potassium aluminum sulfate should be covered during transportation to prevent sun exposure, rain, moisture, and heat. It should not be mixed with toxic, harmful, colored, and easily dyed substances to prevent pollution.
6.4 Industrial potassium aluminum sulfate should be stored in a cool, dry, and ventilated warehouse to prevent rain, moisture, sun exposure, heat, and mixed storage with toxic, colored, and easily dyed substances to prevent pollution.
Additional Notes:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Pingyang Alum Mine in Zhejiang, and Lujiang Alum Mine in Anhui. The main drafters of this standard are Liu Shuying, Ye Xuexi, Zhou Xibao, Xu Jingyuan and Xiang Shanming.4 Industrial aluminum potassium sulfate should be stored in a cool, dry, ventilated warehouse to prevent rain, moisture, sunlight, heat, and mixing with toxic, colored, and easily dyed substances to prevent pollution.
Additional Notes:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Pingyang Alum Mine in Zhejiang, and Lujiang Alum Mine in Anhui. The main drafters of this standard are Liu Shuying, Ye Xuexi, Zhou Xibao, Xu Jingyuan, and Xiang Shanming. 537
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