Some standard content:
Chemical Industry Standard of the People's Republic of China
Water Treatment Agent
Subject Content and Scope of Application
Polyferric Sulfate
HG/T 2153
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation, storage and safety requirements of polyferric sulfate products. This standard applies to liquid polyferric sulfate made from ferrous sulfate and sulfuric acid (including waste acid from sulfuric acid pickling). As a water purifier, this product can be used for the pretreatment of industrial water and the treatment of industrial wastewater, urban sewage and sludge. Molecular formula: [Fc2(OH),(SO)3-m
Cited standards
GB 6678
GB6682
3 Technical requirements
Dangerous goods packaging marking
Pictorial marking for packaging storage and transportation
Preparation of standard solution for titration analysis (volume analysis) Chemical reagents
Chemical reagents
Preparation of standard solution for impurity determination
Preparation of preparations and products used in test methods Chemical reagents
General rules for sampling of chemical products
Specifications for water used in laboratories
3.1 Appearance: reddish brown liquid, without precipitation. 3.2 Polyferric sulfate shall meet the requirements of Table 1. Table 1
Density·g/cm2 (20℃)
Total iron content, %
Reducing substances (as Fe2+) content, %
Basicity, %
pH (1% aqueous solution)
4 Test method
Qualified products
In the test method, unless otherwise specified, only analytically pure reagents and grade 3 water in accordance with the provisions of GB6682 shall be used. Standard solutions, preparations and products required in the test shall be prepared in accordance with the provisions of GB601 and GB603 unless otherwise specified. 4.1 Determination of density (densitometer method)
4.1.1 Summary of the method
The density of the liquid is read from the depth of the densitometer immersed in the liquid when it reaches equilibrium. Approved by the Ministry of Chemical Industry of the People's Republic of China on September 16, 1991 and implemented on January 1, 1992
4.1.2 Instruments and equipment
HG/T 2153- 91
4.1.2.1 Densitometer: scale value is 0.001g/cm*; 4.1.2.21
Constant temperature water bath: can control the temperature at 20℃±1C; 4.1.2.3 Thermometer: scale value is 1C;
4.1.2.4 Graduated cylinder: 250~500ml.
4.1.3 Determination steps
Pour the polyferric sulfate sample into a clean, dry measuring cylinder without any bubbles. Place the measuring tube in a constant temperature water bath at 20°C±1 (. When the temperature is constant, slowly place the density meter into the sample. When the density meter is stable in the sample, read the scale at the lower edge of the meniscus of the density meter (except for the density meter with a scale for reading the upper edge of the meniscus), which is the density of the sample at 20°C. 4.2 Determination of total iron content
4.2.1 Potassium dichromate method
4.2.1.1 Summary of the method
In an acidic solution, stannous chloride is used to reduce ferric iron to ferrous iron. Excess stannous chloride is removed with mercuric chloride, and then titrated with potassium dichromate standard titration solution.
The reaction equation is:
2Fe3++Sn2:-2Fe2++Snt*
SnCl2+2HgCl, = SnCl +Hg,C12
6Fe2++Cr20-+14H+-6Fe3++2Cr3++7H04.2.1.2 Reagents and solutions
Stannoic chloride (GB638) solution: 250g/L hydrochloric acid solution; weigh 25.0g stannous chloride and place it in a dry beaker, dissolve it in 20mL hydrochloric acid (GB622), cool it and dilute it to 100ml and store it in a brown bottle, add a few high-purity tin particles. b.
Hydrochloric acid (GB622) solution: 1+1 solution; mercuric chloride (HG3--1068) saturated solution; sulfur-phosphorus mixed acid;
Dissolve 150ml sulfuric acid (GB625) in 500mL water, add 150mL phosphoric acid (GB1282), and then dilute to 1000mL.
Standard titration solution of potassium dichromate (GB642): c (K, CrzO,) -0. 1mol/L;bzxZ.net
f. Sodium aniline sulfonate (HG3-621) solution: 5g/L. 4.2.1.3 Analysis steps
Weigh about 1.5g of sample, accurate to 0.001g, place in a 250mL conical flask, add 20mL of water, add 20ml of hydrochloric acid solution (4.2.1.2.b), heat to boiling, add stannous chloride solution (4.2.1.2.a) while hot until the yellow color of the solution disappears, add one more drop, cool quickly, add mercuric chloride solution (4. 2.1.2.c) 5mL, shake well and let stand for 1min, then add 50mL of water, then add 10ml of sulfur-phosphorus mixed acid (4.2.1.2.d), 4~5 drops of sodium diphenylamine sulfonate indicator solution (4.2.1.2.f), and titrate with potassium dichromate standard titration solution (4.2.1.2.e) until purple (does not fade after 30s) is the end point.
4.2.1.4 Expression of analysis results
The total iron content X expressed as mass percentage is calculated according to formula (1): V : cX0. 055 85 ×100
Wherein: V is the volume of potassium dichromate standard titration solution consumed by the sample at the stoichiometric point, mL, the concentration of potassium dichromate standard titration solution, mol/I; m--
the mass of the sample·g;
0.05585-·the mass of iron equivalent to 1.00ml of potassium dichromate standard titration solution cg356
-K, Cr0,)-1.000mol/l.
The result should be expressed to the decimal place.
4.2.2 Titanium trichloride method
4.2.2.1 Method summary
HG/T 2153-: 91
Titanium trichloride solution is added dropwise to the acidic solution to reduce the trivalent iron ions to divalent iron ions. The excess titanium trichloride further reduces the sodium dove acid indicator solution to form "tungsten blue", making the solution blue. Under the catalysis of copper salt, with the help of dissolved oxygen in water, the excess titanium trichloride is oxidized. After the blue color of the solution disappears, sodium aniline sulfonate is used as the indicator solution and potassium dichromate standard titration solution is used for titration. The reaction equation is:
Fe+-- Ti+ --- Fe++- Ti+
6Fe\++Cr20-+14H+=6Fe3++2Cr++7H,0Reagents and solutions
Hydrochloric acid (GB622) solution: 1+1 solution;
Sulfuric acid (GB625) solution: 1+1 solution;
Phosphoric acid (GB1282) solution: 15+85 solution; Copper sulfate (GB665) solution: 5g/L;
Titanium trichloride solution: measure 25ml15% titanium trichloride solution, add 20ml hydrochloric acid (GB622), dilute with water to e.
100ml, mix, store in a brown bottle, add a thin layer of liquid paraffin on the solution for protection, it can be used for about 15d. Sodium tungstate solution: 25g/lL, weigh 2.5g sodium tungstate, dissolve in 70ml water, add 7mL phosphoric acid (GB1282). After cooling, dilute with water to 100ml, mix, and put in a brown bottle; -K,Cr:O,) = 0. 015mol/L;
g. Potassium dichromate (GB642) standard titration solution: c(→h. Sodium triphenylamine sulfonate solution (same as 4.2.1.2.f). 4.2.2.3 Analysis steps
Weigh about 0.2~~0.3g of sample, accurate to 0.0001g. Place in a 250mL conical flask, add 10ml of hydrochloric acid solution (4.2.2.2a), 10mL of sulfuric acid solution (4.2.2.2b) and 1mL of sodium tungstate indicator solution (4.2.2.2f). Under continuous shaking, add titanium trichloride solution (4.2.2.2e) drop by drop until the solution just comes out. Until the blue color appears. Rinse the inner wall of the conical flask with water and dilute to about 150mL, add 2 drops of copper sulfate solution (4.2.2.2d), shake thoroughly, and when the blue color of the solution disappears, add 10ml of phosphoric acid solution (4.2.2.2c) and 2 drops of sodium diphenylamine sulfonate indicator solution (4.2.2.2h), and immediately titrate with potassium dichromate standard titration solution (4.2.2.2g) until purple (does not fade after 30s) is the end point. 4.2.2.4 Expression of analysis results
Total iron content X expressed as mass percentage, calculated according to formula (2). X,
武中：V
V: cX 0.055 85×100
The volume of potassium dichromate standard titration solution consumed by the sample at the chemical quantification point, mL;.The concentration of potassium dichromate standard titration solution, mol.l/L.The mass of the sample.
0.05585- and 1.00mL potassium dichromate standard titration solution Cc (mass.
The result should be expressed to two decimal places.
4.2.3 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result; the absolute difference between the two results of the same determination shall not exceed 0.1%; (2)
-KCr20,）=1.000mol/L is equivalent, and the absolute difference in grams of iron determined by different laboratories shall not exceed 0.15%. 4.3 Determination of reducing substance (as Fe2+) content 3.7
4.3.1 Summary of method
HG/T 2153 --- 91
Titrate in acidic solution with potassium permanganate standard titration solution. The reaction equation is:
Mn0,+5Fe2++8H+=Mn2++5Fe++4H,04.3.2 Reagents and solutions
4.3.2.1 Sulfuric acid (GB625);
4.3.2.2 Phosphoric acid (GB1282);
4.3.2.3 Potassium permanganate (GB643) standard titration solution: c (=KMnO,) = 0. 1 mol/L;
4.3.2.4 Potassium permanganate standard titration solution: Dilute the potassium permanganate standard titration solution in 4.3.2.3 by 10 times, prepare it as needed, and use it on the same day.
4.3.3 Instruments and equipment
4.3.3.1 Microburette, 1mL.
4.3.4 Analysis steps
Weigh about 5g of sample, accurate to 0.001g, place in a 250ml conical flask, add 150ml of water, add 4ml of sulfuric acid (GB625), 4ml of phosphoric acid (GB1282), shake well. Titrate with potassium permanganate standard titration solution (4.3.2.4) until it turns slightly red (does not fade after 30s), which is the end point. Perform a blank test at the same time.
4.3.5 Expression of analysis results
The content of reducing substances (in terms of Fe2+) expressed in mass percentage X is calculated according to formula (3): X.=
(VV。): cX0. 055 85
Wherein: V---the volume of potassium permanganate standard titration solution (4.3.2.4) consumed by the sample at the stoichiometric point, mL. V。 --- Volume of potassium permanganate standard titration solution (4.3.2.4) consumed by the blank at the stoichiometric point, mL. =-Concentration of potassium permanganate standard titration solution (4.3.2.4), mol/L; m-mass of the sample. g;
0.05585--Mass of iron in grams equivalent to 1.00mL potassium permanganate standard titration solution (c(÷KMnO,)=1.000mol/L>).
The result should be expressed to two decimal places.
4.3.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result; the absolute difference between the two parallel determination results shall not exceed 0.01%; the absolute difference between the determination results of different laboratories shall not exceed 0.02%. 4.4 Basicity determination
4.4.1 Summary of method
Add a certain amount of hydrochloric acid solution to the sample, then add potassium fluoride to mask the iron, and then add sodium hydroxide to Titration with standard titration solution. 4.4.2 Reagents and solutions
4.4.2.1 Hydrochloric acid (GB622) solution: 1+3 solution; 4.4.2.2 Sodium hydroxide (GB629) solution: c(NaOH)-0.1mol/L solution; 4.4.2.3 Hydrochloric acid (GB622) solution: c(HCI)-0.1mol/L solution; 4.4.2.4 Potassium fluoride (GB1271): 500g/L solution. Weigh 500g potassium fluoride, dissolve it in 200mL distilled water without carbon dioxide, dilute to 1000mL, add 2mL phenolphthalein indicator and adjust the solution with sodium hydroxide solution (4.4.2.2) or hydrochloric acid solution (4.4.2.1) until it is slightly red, filter out the insoluble matter and store in a plastic bottle.
HG/T 2153-- 91
4.4.2.5 Sodium hydroxide (GB629): c (NaOH) = 0.1 mol/L standard titration solution 4.4.2.6 Phenolphthalein (GB10729): 10 g/I. ethanol solution. 4.4.3 Analysis steps
Weigh about 1.5 g of sample, accurate to 0.001 g, place in a 250 ml conical flask, use a pipette to accurately add 25.00 ml of hydrochloric acid solution (4.4.2.3), add 20 ml of boiled and cooled distilled water, shake Cover the surface IIIl evenly. Leave at room temperature for 10 minutes, then add 10mL of potassium fluoride solution (4.4.2.4), shake well, add 5 drops of phenol indicator (4.4.2.6), and immediately titrate with sodium hydroxide standard titration solution (4.4.2.5) until the color turns light red (does not fade after 30 seconds) as the end point. At the same time, use boiled and cooled distilled water instead of the sample for a blank test. 4.4.4 Expression of analysis results
The basicity Xs expressed as mass white fraction is calculated according to formula (4): (V.-V) : cX0.017 0
(V.-V) : cX0. 018 62
-The volume of the standard sodium hydroxide titration solution consumed by the blank test at the stoichiometric point, mL; V.—
The volume of the standard sodium hydroxide titration solution consumed by the sample at the stoichiometric point, mL; The concentration of the standard sodium hydroxide titration solution, mol/L; The mass of the sample, g;
(4)
X——The mass percentage of trivalent iron in the sample, X,=X1-X: or X—Xz—X3, 0.0170—The mass of hydroxyl (OH-) in grams equivalent to 1.00mL of the standard sodium hydroxide titration solution Cc (NaOH)=1.000mL./L].
:-The molar mass of iron (→Fe)·g/mol. The result should be expressed to two decimal places.
4.4.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result; the absolute difference between the two parallel determination results shall not exceed 0.2%; the absolute difference between the determination results of different laboratories shall not exceed 0.5%. 4.5 Determination of pH value
4.5.1 Reagents and solutions
4.5.1.1 Potassium hydrogen phthalate pH standard solution with pH=4.00: 4.5.1.2 Potassium dihydrogen phosphate-potassium hydrogen phthalate pH standard solution with pH=6.86. 4.5.2 Instruments and equipment
4.5.2.1 Acidity meter: accuracy 0.1pH;
4.5.2.2 Glass electrode;
4.5.2.3 Saturated calomel electrode.
4.5.3 Determination steps
4.5.3.1 Preparation of sample solution
Weigh 1.0g of sample and place it in a beaker, dilute with water, transfer all to a 100mL volumetric flask and dilute to the scale, shake well. 4.5.3.2 Determination
After positioning with buffer solutions of pH=4.00 and pH=6.86, pour the sample solution (4.5.3.1) into the beaker, immerse the saturated calomel electrode and the glass electrode in the solution to be tested, and read the value when the pH value is stable (the change in pH value within 1 minute is not greater than 0.1). 5 Inspection rules
5.1 Polyferric sulfate should be inspected by the quality inspection department of the manufacturer in accordance with the test methods and inspection rules specified in this standard. The manufacturer should ensure that all products leaving the factory meet the requirements of this standard. 5.2 Each batch of the factory's products should be accompanied by a quality manual, including: manufacturer name, product name, grade, batch number, production date, net weight, certificate of product quality compliance with this standard and the number of this standard. 5.3 The user has the right to conduct quality inspections on the products received in accordance with the provisions of this standard to verify whether their quality meets the requirements of this standard.
5.4 Each can is a batch, and each batch is not less than 10t. 5.5 When sampling, use a glass tube or plastic tube to insert 2/3 of the storage tank to take out the sample. The sample taken out is not less than 500ml. Put it into two clean and dry bottles respectively, seal the bottle mouth, and put labels on the bottles, indicating the manufacturer name, product name, product batch number, and sampling date. One bottle will be inspected by the quality inspection department, and the other bottle will be kept as a reserved sample for inspection, and the retention period is six months. 5.6 If one of the inspection results does not meet the requirements of this standard, double the sample should be drawn for re-inspection. If one of the inspection results does not meet the requirements of this standard, the entire product will be rejected. 5.7 When the supply and demand parties have disputes over product quality, they can handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 6 Marking, packaging, transportation, storage
6.1 Polyferric sulfate is packaged in glass fiber reinforced plastic tank trucks or iron barrels lined with plastic barrels. 6.2 The package should be accompanied by a product certificate, which includes: product name, manufacturer name, indicators, batch number, net weight, production date and this standard number.
6.3 Polyferric sulfate is corrosive. The packaging container should be painted with the corrosive item mark specified in GB190 and the upward and heat-resistant marks specified in GB191.
6.4 Do not expose to sunlight during storage. The storage temperature should not be lower than -20°C. The effective storage period is half a year. 7 Safety requirements
Polyferric sulfate products are corrosive and irritating to a certain extent. Operators should wear protective equipment to avoid direct physical contact when performing operations.
Additional instructions:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical supervision of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Chemical Research Institute of the Ministry of Chemical Industry and Hangzhou Sulfuric Acid Research Institute. The main drafters of this standard are Shao Weiren, Dai Siyan, Zhu Chuanjun, Shan Qi and Zhao Jiming.
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