Some standard content:
National Standard of the People's Republic of China
Water
Treatment
Ferrous sulfate
Water treatment chemicals
Fertous sulphate
Theme content and scope of application
Agent
GB 10531 - 89
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of water treatment agent ferrous sulfate. This standard applies to water treatment agent ferrous sulfate. This product is mainly used for the treatment of drinking water and industrial water. Molecular formula: FeSO7H20
Molecular weight: 278.01 (according to the 1985 international atomic weight) reference standard
2
GB 601
GB 602
GB603||tt| |GB 610bZxz.net
GB3049
GB 6678
3 Technical requirements
Preparation of standard solutions for chemical reagent titration analysis (volume analysis) Chemical reagents
Impurities Preparation of standard solutions for determination
Preparation of preparations and products used in chemical reagent test methods General method for determination of chemical reagents arsenic (arsenic spot method) General method for determination of iron content in chemical products Orthopheneline spectrophotometry Chemical products General Sampling Principles
3.1 Appearance: light green or light yellow-green crystal. 3.2 The water treatment agent ferrous sulfate should meet the requirements of Table 1. Table 1
refers to
refers to
standard item
ferrous sulfate (FeSO·7H20) content, % oxidation sensitive (TiO2) content, %
Water-insoluble matter content, %
Free acid (calculated as H2SO) content, %
Arsenic (As) content, %
Heavy metal (calculated as Pb) content, %||tt ||Superior product
97.0
0.5
0.2
0.35
For drinking water treatment
First-class product
94.0 | |tt||0.002
Qualified product
90.0
0.75
0.75
2. 0
0.0005
0.002
Standard
For industrial water treatment
High-quality products
97.0
0. 5
0. 2
etc. Product
94.0
0.5
0.5
Qualified product
90.0
0.75
0.75
1989 -12-01 Implementation
311
4 test methods
GB 10531-89
The reagents and water used in this standard refer to Analytical grade reagents and distilled water or water of corresponding purity. The standard solutions, impurity standard solutions, preparations and products required in the test shall be prepared in accordance with the provisions of GB601, GB602 and GB603 unless otherwise specified
4.1 Determination of ferrous sulfate (FeSO4·7H20) content 4.1. 1 Principle
In acidic medium, titrate with potassium permanganate to oxidize ferrous iron into trivalent iron, and use the titrant itself to indicate the end point. 4.1.2 Reagents and solutions
Sulfuric acid (GB625): 1→1 solution;
a.
b. Phosphoric acid (GB1282): 1+1 solution;
Potassium permanganate (GB643): c (1/5KMnO.) about 0.1mol/L standard solution. c.
4.1.3 Measurement Procedure
Weigh about 1g of sample, accurate to 0.0002g. Place in a 300mL Erlenmeyer flask. Dissolve in 50mL water. Add 10mL sulfuric acid (4.1.2a) and 4mL phosphoric acid (1.1.2b). Titrate with potassium permanganate standard solution (4.1.2c) until the pink color of the solution does not disappear within 30 seconds, which is the end point.
4.1.4 Expression and calculation of results
The ferrous sulfate (FeSO,·7H2O) content (X1) expressed as a mass percentage is calculated according to formula (1): V: c× 0.278 0 × 100 =
The volume of potassium permanganate standard solution (4.1.2c) consumed by the titration sample, mL; the concentration of potassium permanganate standard solution (4.1.2c), mo1/L; (1)
-1.00mL Potassium permanganate standard solution [c (1/5KMnO.) = 1.000mol/L is equivalent to the mass of ferrous sulfate, g; sample mass, name.
The difference between the results of two parallel measurements shall not be greater than 0.4%. Take the arithmetic mean as the measurement result. 4.2 Determination of titanium dioxide (TiO2) content
4.2.1 Principle
Dissolve the sample with dilute sulfuric acid, add sulfur-phosphorus mixed acid and hydrogen peroxide to develop color, and measure the absorbance using spectrophotometry. 4.2.2 Reagents and solutions
a.
b.
c,
d.
&
f.||tt ||g.
h.
Sulfuric acid (GB625);
Sulfuric acid (GB625): 1+99 solution:
Sulfuric acid (GB625): 1+1 solution ;
Phosphoric acid (GB1282): 1+1 solution;
Titanium dioxide (spectrally pure);
Ammonium sulfate (GB1396);
30% hydrogen peroxide (HG3 --1082): 3% (m/m) solution; ferric ammonium sulfate (GB1279);
i.
Titanium standard solution: 0.2mgTiOz/mL. Weigh 0.2000g titanium dioxide (4.2.2e) and place it in a 250mL beaker. Add 50mL sulfuric acid (1.2.2a) and 30g ammonium sulfate (4.2.2f). Stir thoroughly. Heat slowly and then strongly on the electric furnace until the sample is completely Dissolve. After cooling, transfer to a 1000mL volumetric flask, add water to dilute to the mark. Shake well; Iron standard solution: 2mgFe/mL. Weigh 17.26g of ferric ammonium sulfate (4.2.2h), dissolve it with sulfuric acid solution (4.2.2b), move it into a j.
1000mL volumetric flask, dilute to the mark with sulfuric acid solution (4.2.2b), and shake uniform. 4.2.3 Instruments and equipment
312
General laboratory instruments and
GB 10531 —89
4.2.3.1 Spectrophotometer: with a thickness of 3cm Absorption pool. 4.2.4 Drawing of standard curve
4.2.4.1 Preparation of standard reference solution
In seven 100mL volumetric flasks, add 0 (reagent blank solution), 0.50, 1.00, 2.00, 3.00 respectively. , 4.00.5.00mL titanium standard solution (4.2.2i).
4.2.4.2 Color development
Each volumetric flask is treated in the same manner at the same time according to the following regulations: add water to about 50mL, add 10mL sulfuric acid (4.2.2c), 5mL phosphoric acid (4.2.2d), Shake well. After cooling to room temperature, add 5 mL hydrogen peroxide solution (4.2.2 g) and dilute to volume with water. Shake the hook. 4.2.4.3 Measurement of absorbance
Use a spectrophotometer (4.2.3.1) at a wavelength of 410nm, use a 3cm absorption cell, and use water as a control to measure the absorbance. 4.2.4.4 Drawing of standard curve
Subtract the absorbance of the reagent blank solution from the absorbance of each standard reference solution, take the content of titanium dioxide (mg) as the abscissa, and the corresponding absorbance as the ordinate, draw the standard curve. 4.2.5 Measurement procedures
4.2.5.1 Preparation of test solution
Weigh 5.000:01g sample and place it in a 200mL beaker. After dissolving with sulfuric acid (4.2.2b), transfer it to a 500mL volumetric flask and dilute to the mark with sulfuric acid solution (4.2.2b). Shake well. 4.2.5.2 Preparation of blank test solution
In a 100mL volumetric flask, use a pipette to transfer 10mL iron standard solution (4.2.2i). 4.2.5.3 Color development
Use a pipette to transfer 10mL of test solution (4.2.5.1) and place it in a 100mL volumetric flask. Place the test solution and blank test solution (4.2.5.2) according to 4.2.4.2 respectively. stipulations shall be dealt with in the same manner at the same time. 4.2.5.4 Measurement of absorbance
Use a spectrophotometer (4.2.3.1) at a wavelength of 410nm, use a 3cm absorption cell, and use water as a control to measure the absorbance. 4.2.6 Expression and calculation of results
The titanium dioxide (TiO2) content (X2) expressed as mass percentage is calculated according to formula (2): m×10/500×100= 5mo
ms × 10 -3
TiO. content detected from the standard curve, mg; sample mass, 8.
The difference between the results of two parallel measurements shall not be greater than 0.02%. Take the arithmetic mean as the measurement result. 4.3 Determination of water-insoluble matter content
4.3.1 Reagents and solutions
a.
Sulfuric acid (GB 625);
Sulfuric acid (GB625): 1+99 solution . | |tt | ~15μm. 4.3.3 Measurement procedures
Weigh about 10g of sample, accurate to 0.01g, and place it in a 250mL beaker. Add 200mL water and 2mL sulfuric acid (4.3.1a). Stir. After fully dissolved, filter with a crucible filter (4.3.2.1) that has been constant weight at 105~~110℃. Wash 8~~10 times with sulfuric acid solution (4.3.1b) 313
GB10537 —
89
(about 5mL each time). Then wash with water 8 to 10 times (about 5mL each time). Bake at 105~110C until constant weight. 4.3.4 Representation and calculation of nesting
The water-insoluble content (X:) expressed as mass percentage is calculated according to formula (3): The mass of the filter,
rm2
m: × 100
m
The mass of water-insoluble matter and sugar pot filter·8; m2||tt| |Sample quality,.
(3)
The difference between two parallel measurement results shall not be greater than 0.01% for superior products, and shall not be greater than 0.04% for first-class products and qualified products. Take the arithmetic mean as the measurement result.
4.4 Determination of free acid (calculated as H, SO.) content 4.4.1 Principle
Dissolve the sample in isopropyl alcohol and filter. Use phenolphthalein as indicator and titrate with sodium hydroxide standard solution. 4.4.2 Reagents and solutions
a.
b.
c.
Isopropyl alcohol (HG3-1167);
Sodium hydroxide ( GB629): c (NaOH) about 0.05mol/L standard solution; hydrochloric acid (GB622): 5% (m/m) solution; d.
sodium hydroxide (GB629): 50g/L solution; phenol ( HGB3039): 10g/L ethanol solution; e.
f. Pan-pH test paper;
Pickled asbestos (HG3-1062): Take an appropriate amount of pickled asbestos, add hydrochloric acid solution (4.4.2c) and boil for 20 minutes. Wash with water until neutral [check with test paper (4.4.2f)]. Add sodium hydroxide solution (4.4.2d) and boil for 20 minutes. Wash with water until neutral and check with test paper (4.4.2f)]. Make a thin paste with water and set aside.
4.4.3 Instruments and equipment
-General laboratory instruments and
4.4.3.1 Gouchen crucible: 25mL.
Evenly spread a 1~~2mm thick layer of pickled asbestos (4.4.2g) on ??the upper and lower sides of the Gu's citrus crucible, filter and wash with hot water until the filtrate does not contain asbestos lint. Dry this wax at 105~110℃. 4.4.4 Measurement procedures
Weigh about 5g of sample, accurate to 0.01g, and place it in a 250mL iodine volume bottle. Add 50 mL isopropyl alcohol (4.4.2a) and shake for 10 minutes. Filter using a Cousin's crucible (4.4.3.1). Leave the ferrous sulfate in the bottle if possible. Wash the residue in the bottle = times with 10 mL of isopropyl alcohol (4.4.2a) each time. Finally, wash the Gouchen pot with 10 mL of isopropyl alcohol (4.4.2a). Add 3 to 4 drops of phenolic acid indicator (4.1.2c) to the filtrate. Titrate the filtrate with sodium hydroxide standard solution (1.4.2b) until pink color appears, which is the end point. At the same time, perform a blank test using the same amount of isopropyl alcohol and following the same steps.
4.4.5 Expression and calculation of results
The free acid (based on H2SO) content (X) expressed as mass percentage is calculated according to formula (4): X
rdt.I 'u....
-
0.049 0
t
314
(V -- Va)c × 0. 049 0|| tt|| ; The volume of sodium hydroxide standard solution (4.4.2b) consumed in titrating the test solution, mL; the concentration of sodium hydroxide standard solution (4.4.2b), mo1/L; 1.00mL sodium hydroxide solution [c (Na0H) 1.000 mol/L) is equivalent to the mass of sulfuric acid, g; the mass of the sample, B.
(A
GB 10531-89
The difference between the two parallel measurement results is not greater than 0.05%. The arithmetic mean is taken as the measurement result. 4.5 Determination of arsenic (As) content
4.5.1 Principle
In acidic medium, metallic zinc reduces arsenic compounds to arsenic hydrogen, which forms arsenic spots on the mercury bromide test paper and is compared with standard arsenic spots. .
4.5.2 Reagents and solutions
mother.
d.
e.
f.||tt ||Hydrochloric acid (GB 622);
Potassium iodide (GB1272);
Stannous chloride (GB638): 400g/L hydrochloric acid solution; arsenic-free metallic zinc (GB2304)
Brome Mercury test paper;
Lead acetate cotton;
g
Dioxide trioxide (GB673);
h.
Arsenic standard solution: 0.0010mgAs /mL, prepared according to GB602, diluted 100 times. 4.5.3 Instruments and equipment
General laboratory instruments and
4.5.3.1 Arsenic determiner: use GB610. .1 The device shown in Figure 1. 4.5.4 Measurement procedure
Weigh 1.00±0.01g sample, add 70mL of water to dissolve, then add 6mL of hydrochloric acid (4.5.2a). 1g potassium iodide (4.5.2b), add stannous chloride solution (4.5.2c) dropwise until the solution is colorless, shake well, add 2.5g arsenic-free metallic zinc (4.5.2d), and immediately add acetic acid. Install the lead cotton (4.5.2f) and mercury bromide test paper (4.5.2e) in the dark place for 1 hour. The color of the mercury bromide test paper should not be darker than the standard. Take 5.00mL arsenic standard solution (4.5.2h) and process it in the same way as the sample. 4.6 Determination of heavy metal (calculated as Pb)
4.6.1 Principle
In a weakly acidic medium, The heavy metal ions in the sample react with hydrogen sulfide to form a brown sulfide precipitate. Compare the color of the test solution with the standard color
Sulfuric acid (GB625): 1+. 1 solution;
hydroxylamine hydrochloride (HG 3--967);
b.
c.
saturated hydrogen sulfide water: ready for use;||tt ||Lead standard solution: 0.010mgPb/mL. Prepare according to GB602 and dilute 10 times. d.
4.6.3 Determination procedures
4.6.3.1 Preparation of test solution.
Weigh 5.00±0.01g sample and place it in a 250mL beaker. Dissolve it with 50mL Yonghe 1mL sulfuric acid (4.6.2a) and add 0.5g hydroxylamine hydrochloride (4.6.2b), boil for 1 minute and cool to room temperature. Transfer all to a 100mL volumetric flask. Dilute to volume and shake well. Dry filter if necessary.
4.6.3.2 Determination
Use a pipette to transfer 40mL of test solution (4.6.3.1) and place it in a 50mL colorimetric tube. Use a pipette to transfer 20mL of the test solution (4.6.3.1) into another colorimetric tube, and add 2.00mL of lead standard solution (4.6.2d) as the standard. Add 10mL of saturated hydrogen sulfide water (4.6.2c) respectively. Dilute to volume with water and shake well. Color comparison within 2 minutes. The color of the test solution shall not be darker than the standard. 315
5 Inspection Rules
GB10531-89
5.1 The water treatment agent ferrous sulfate should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that each batch of products meets the requirements of this standard.
5.2 The user has the right to conduct quality inspection of the products received in accordance with the provisions of this standard. Check whether it meets the requirements of this standard. 5.3 The weight of each batch of products shall not exceed 60t.
5.4 Sampling method: For bagged products, the number of sampling bags is determined according to Table 2. Table 2
Total number of bags in each batch
1～10
J149
50~64
65~81
82~~ -101
102~~125
126~151
The minimum number of sampling bags selected
The total number of bags
1
12
13
14
15
16
Total number of bags per batch
152~181
182~216
217~254
255~296
297~343
344 ~ 394
395--450
The minimum sample selected Number of bags
17
18
19
20
21
22
23
will The sampler is inserted into the material layer three-quarters of the way to take samples. Take about 100 per bag. For bulk products, samples should be taken from 10 sampling points evenly distributed on the bulk area of ??the product, and the sample taken at each point should not be less than 100g. Mix the sample taken quickly. Divide into 500g according to the quartering rule and pack into two clean, dry bottles with ground stoppers. Put a label on the bottle, indicating: manufacturer name, product name, grade, batch number and sampling date. - One bottle is sent to the inspection department for inspection, and the other bottle is kept for one week for future reference. 5.5 If any indicator in the inspection results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging or sampling points for verification. If even one indicator does not meet the requirements of this standard as a result of the re-inspection, the entire batch of products will not be accepted. 5.6 When the supply and demand parties have objections to product quality, they shall be handled in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration and Inspection". 6 Marking, packaging, transportation and storage
6.1 The water treatment agent ferrous sulfate is lined with plastic bags and double-packed in woven bags. The inner bag is tied (or heat-sealed) and the outer bag should be firmly sealed. This product is also available in bulk.
6.2 The name of the manufacturer, product name, production date, batch number, net weight, trademark and this standard number should be marked on the packaging bag. Net weight of each bag is 50kg. Bulk products should indicate the above on the loading list. 6.3 Care should be taken during shipment to prevent damage to the packaging. It should not be exposed to the sun or rain, and it is prohibited to store or transport it with toxic and harmful substances. Additional notes:
This standard is under the jurisdiction of the Tianjin Chemical Industry Research Institute of the Ministry of Chemistry and Industry. This standard is drafted by the Tianjin Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Zhou Qiao'e and Wang Qi. This standard refers to the American Water Works Association AWWAB402--85 "Ferous Sulfate". 316
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