Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2528-93
Trisodium Phosphate Chloride
Published on September 8, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1994
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG2528-93
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of trisodium phosphate chloride. This standard applies to trisodium phosphate chloride synthesized from raw materials such as thermal phosphoric acid, sodium hydroxide, and liquid chlorine. This product is mainly used in disinfection, washing, and detergent compounding departments. Molecular formula: (NasPO·11H20)NaCI0
Relative molecular mass: 1523.08 (according to the international atomic weight in 1989) 2 Reference standards
GB/T601 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T602 Chemical reagents
Preparation of standard solutions for determination of impurities
GB/T603
Preparation of preparations and products used in test methods for chemical reagents GB/T610 .1 Chemical reagents General method for determination of arsenic (arsenic spot method) GB1250
Expression and determination method of limit values Corrugated paperboard
GB6543
GB/T6678
General rules for sampling of chemical products
GB/T6682 Specifications and test methods for water used in analytical laboratories GB8946
Plastic textile bags
Technical requirements
3.1 Appearance: This product is white crystals or crystalline powder. 3.2 Trisodium phosphate chloride shall meet the requirements of the following table Item
Available chlorine (as C1) content, %
Phosphorus pentoxide (P20) content, %
Arsenic (As) content, %
Heavy metal (as Pb) content, %
pH value (10g/L solution)
Approved by the Ministry of Chemical Industry of the People's Republic of China on September 8, 1993
First-class product
11.6~11.8
Qualified product
Implemented on July 1, 1994
W.bzsoso:com4 Test method
HG/T2528-93
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682. The standard titration solution, impurity standard solution, preparation and product required in the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified. 4.1 Determination of effective chlorine content
4.1.1 Summary of method
The sample is reacted with potassium iodide under acidic conditions, and the precipitated iodine is titrated with sodium thiosulfate standard titration solution. Starch is used as an indicator, and the effective chlorine content is determined based on the consumption of sodium thiosulfate standard titration solution. 4.1.2 Reagents and materials
4.1.2.1 Potassium iodide (GB/T1272);
4.1.2.2 Glacial acetic acid (GB/T676): 1+1 solution; 4.1.2.3 Sodium thiosulfate (GB/T637): c (NazS20s) is about 0.1mol/L standard titration solution; 4.1.2.4 Soluble starch: 5g/L indicator solution. 4.1.3 Analysis steps
Weigh about 2g of sample, accurate to 0.0002g, put it in an iodine volumetric bottle, add 50mL of water to dissolve, add 2g of potassium iodide and 30mL of acetic acid solution, shake the hook, place it in a dark place for 10min, add 100mL of water, titrate with sodium thiosulfate standard titration solution, add 3mL of starch indicator solution when it is close to the end point, and continue to titrate until the blue color just disappears. At the same time, perform a blank test. 4.1.4 Expression of analysis results
The content of available chlorine (in terms of CI) expressed as mass percentage (X1) is calculated according to formula (1): (VV)·cX0. 035 45×100
3. 545× (V-Vo)Xc
Wherein: V is the volume of sodium thiosulfate standard titration solution consumed in titrating the test solution, mL; V is the volume of sodium thiosulfate standard titration solution consumed in titrating the blank solution, mL; c is the actual concentration of sodium thiosulfate standard titration solution, mol/L; m is the mass of the sample, g;
0.03545 is the mass of available chlorine (in terms of CI) in grams equivalent to 1.00 mL of sodium thiosulfate standard titration solution [c (Na2S20s) = 1.000 mol/L].
4.1.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference between two parallel determinations shall not exceed 0.05%. 4.2 Determination of phosphorus pentoxide content
4.2.1 Method summary
In nitric acid medium, the sample and the added quinoline molybdate precipitant generate quinoline phosphomolybdate precipitate. After filtering, drying and weighing, the phosphorus pentoxide content is determined.
4.2.2 Reagents and materials
4.2.2.1 Nitric acid (GB/T626): 1+1 solution; 4.2.2.2 Quinoline molybdate solution.
Preparation: (a) Weigh 70g sodium molybdate (Na2Mo02·H2O) (HG3-1087) and dissolve it in 150mL water; 2
HG/T2528—93
(b) Weigh 60g citric acid (CsHgOz·H20) (GB9855) and dissolve it in a mixture of 150mL water and 85mL nitric acid (GB/T626);
(c) Add solution (a) to solution (b) under stirring; (d) Add 35mL nitric acid (GB/T626) and 5mL quinone to 100mL water; (e) Add solution (d) to solution (c), let it stand for 12h, filter it with a crucible filter, add 280mL acetone (GB/T686), dilute it to 1000mL with water, mix well, store it in a polyethylene bottle, and keep it in a dark place. 4.2.3 Instruments: Equipment
4.2.3.1 Filter: pore size of filter plate 515μm, 4.2.3.2 Electric oven: temperature can be controlled at 180±5℃ or 250±10℃. 4.2.4 Analysis steps
4.2.4.1 Preparation of test solution
Weigh about 5g of sample, accurate to 0.0002g, put it in a 100mL beaker, add 20mL of water to dissolve, add 5mL of nitric acid solution, heat to a slight boil, wait until the solution is reduced to 10mL, cool, transfer all into a 250mL volumetric flask, dilute with water to the scale, shake well, dry filter with medium-speed filter paper into a conical flask (discard the first 20mL of filtrate), which is the test solution. 4.2.4.2 Preparation of blank test solution
When preparing the test solution, except for not adding the sample, other operations and the amount of reagents added are handled in the same way as the test solution. 4.2.4.3 Determination
Use a pipette to transfer 10 mL of test solution and blank test solution into a 250 mL beaker respectively. Add 15 mL of nitric acid solution and 80 mL of water. Then add 50 mL of quinoline molybdate solution. Cover with a watch glass and heat in a water bath until the solution in the beaker reaches 75 ± 5°C for 30 seconds (do not use open flames or stir during the addition of reagents and heating to avoid caking). Take it out and cool it to room temperature. During the cooling process, stir it 3 to 4 times. Filter it with a filter that has been pre-conditioned at 180 ± 5°C or 250 ± 10°C. Filter the supernatant first, rinse the precipitate 6 times with a washing bottle by decantation method, using about 30 mL of water each time. Finally, transfer the precipitate to a crucible filter and wash it with water 4 times. Place the crucible filter together with the precipitate in an electric oven. Start timing after the temperature stabilizes. Control the temperature at 180 ± 5°C and dry it for 45 minutes, or at 250 ± 10°C and dry it for 15 minutes. Take it out, place it in a desiccator, cool it to room temperature, and weigh it. 4.2.5 Expression of analysis results
The content of phosphorus pentoxide (P2Os) (X2) expressed as mass percentage is calculated according to formula (2):_(m1mo)X0. 032 07×100
m×250
80.2(ml-mo)
Wherein: m1——mass of quinoline phosphomolybdic acid precipitate generated in the test solution, g; mo—mass of quinoline phosphomolybdic acid precipitate generated in the blank test solution, g; m—mass of the sample, g;
0.03207——coefficient for converting quinoline phosphomolybdic acid into phosphorus pentoxide. 4.2.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between two parallel determinations shall not exceed 0.2%. 4.3 Determination of arsenic content
4.3.1 Method Summary
In an acidic solution, potassium iodide and stannous chloride are used to reduce high-valent arsenic to trivalent arsenic. Trivalent arsenic reacts with new ecological hydrogen to generate arsenic hydrogen gas, which forms a brown-yellow arsenic spot on the mercuric bromide test paper, which is compared with the standard color spot. 3
W.bzsosO.cO4.3.2 Reagents and materialsWww.bzxZ.net
4.3.2.1 Arsenic-free metallic zinc (GB/T2304); HG/T2528-93
4.3.2.2 Hydrochloric acid (GB/T622): 1+1 solution; 4.3.2.3 Potassium iodide (GB/T1272): 150g/L solution; 4.3.2.4 Stannous chloride (GB/T638): 400g/L solution; 4.3.2.5 Lead acetate (HG3-974) cotton, 4.3.2.6 Mercuric bromide (GB/T1398) test paper; 4.3.2.7 Arsenic standard solution: 1mL contains 0.010mgAs. Prepare before use. Use a pipette to transfer 10mL of the standard solution prepared according to GB/T602, place it in a 100mL volumetric flask, dilute it with water to the mark, and shake it well.
4.3.3 Instruments and equipment
4.3.3.1 Analyzer: See Article 5 of GB/T610.1. 4.3.4 Analysis steps
Weigh about 1g of sample, accurate to 0.01g, place it in a 150mL beaker, add 10mL of water and 5mL of hydrochloric acid solution, heat to boiling, keep it at a slight boil for 5min, and cool it. Transfer all of it to the arsenic determination bottle, add water to a total volume of about 40mL, add 20mL of hydrochloric acid solution, and shake it well. Add 5mL of potassium iodide solution and 1mL of stannous chloride solution, and shake it well. Let it stand at room temperature for 10min. Then add 2.5g of arsenic-free metal zinc, immediately plug the arsenic determination tube pre-filled with lead acetate cotton and mercuric bromide test paper, and place it in the dark for 1h. Take out the mercuric bromide test paper, and the arsenic spot should not be darker than the standard spot.
The standard spot is to use a pipette to transfer 1mL (first-class product) or 5mL (qualified product) of the arsenic standard solution and treat it in the same way as the test sample. 4.4 Determination of heavy metal content
4.4.1 Method summary
In a weakly acidic solution, heavy metal ions and divalent sulfide ions form colored sulfide precipitates. When the heavy metal ion content is low, a stable dark suspension is generated, which can be used for visual colorimetric determination of heavy metals. 4.4.2 Reagents and materials
4.4.2.1 Nitric acid (GB/T626): 1+1 solution; 4.4.2.2 Ammonia water (GB/T631): 2+3 solution; 4.4.2.3 Glacial acetic acid (GB/T676): 1+1 solution; 4.4.2.4 Saturated hydrogen sulfide water: prepare before use; 4.4.2.5 Lead standard solution: 1mL contains 0.010mgPb. Prepare before use Use a pipette to transfer 10mL of the lead standard solution prepared according to GB/T602, place it in a 100mL volumetric flask, dilute to the mark with water, and shake well.
4.4.3 Analysis steps
4.4.3.1 Preparation of test solution
Weigh about 1g of sample, accurate to 0.01g, place in a 150mL beaker, add 10mL water and 1mL nitric acid solution, heat to boiling, keep boiling for 5min, and cool. Add 10mL water and 0.5mL nitric acid solution, and adjust pH to 5 with ammonia water (check with precision test paper). 4.4.3.2 Determination
Transfer all the test solution to a 50mL colorimetric tube, add 0.5mL acetic acid solution, add water to about 40mL, add 10mL saturated hydrogen sulfide water, shake well, and place in a dark place for 10min. The color should not be darker than the standard colorimetric solution. The standard colorimetric solution is to take 1mL (first-class product) and 5mL (qualified product) of the lead standard solution with a pipette and treat it in the same way as the sample.
4.5 Determination of pH value
W.bzsoso.coI4.5.1 Summary of method
HG/T2528-93
Immerse the indicator electrode and the reference electrode in the test solution to form a primary cell, whose electromotive force is related to the pH value of the solution. By measuring the electromotive force of the primary cell, the pH value of the solution can be obtained. 4.5.2 Instruments and equipment
4.5.2.1 Acidometer: accuracy is 0.1 pH unit; 4.5.2.2 Glass electrode: must be soaked in water for more than 24 hours before use and stored in water; 4.5.2.3 Saturated calomel electrode.
4.5.3 Analysis steps
Weigh about 1g of sample, accurate to 0.1g, place it in a 250mL beaker, add 100mL of water to dissolve, and use a calibrated acidometer to determine the pH value of the solution.
To ensure the accuracy of the measured results, the acidometer and the test solution can be repeatedly calibrated until the pH reading is stable for at least 1 minute. 5 Inspection rules
5.1 Trisodium phosphate chloride should be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer should ensure that all trisodium phosphate chloride products shipped out of the factory meet the requirements of this standard. Each batch of trisodium phosphate chloride shipped out of the factory should be accompanied by a quality certificate. The content includes: manufacturer name, product name, grade, net weight, batch number or production date, product quality certification that meets this standard and this standard number. 5.2 The user unit has the right to accept the received trisodium phosphate chloride products in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 5t.
5.4 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB/T6678. Each box or each plastic woven bag is a packaging unit. When sampling, take out no less than 50g of sample from each selected packaging unit, mix the sample, and then divide it into about 500g by quartering method, and immediately put it into two clean and dry wide-mouth bottles with ground stoppers and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler. One bottle is inspected by hand, and the other bottle is kept for 3 months for future reference. 5.5 If one indicator of the inspection result does not meet the requirements of this standard, sampling should be carried out from twice the amount of packaging. Even if only one indicator of the inspection result does not meet the requirements of this standard, the whole 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 "Interim Measures for National Product Quality Arbitration Inspection". The rounded value comparison method specified in GB1250 shall be used to determine whether the inspection results meet the standards. 6 Marking, packaging, transportation, storage
6.1 The packaging bags and boxes of trisodium phosphate chloride should be firmly and clearly marked, including: manufacturer name, product name, trademark, grade, net weight, batch number or production date and this standard number, as well as "Mark 7 Moisture-averse Mark" in GB191. 6.2 Trisodium phosphate chloride is packaged in two ways 6.2.1 Double corrugated carton and plastic bag packaging. The inner packaging is a polyethylene plastic film bag with specifications and dimensions: 270mm×180mm or 180mm×135mm or 70mm×40mm, thickness of 0.05mm, net weight of each bag 500g or 250g or 50g. The outer packaging is a double corrugated carton with specifications and dimensions: 440mmX290mm×260mm, and its performance and inspection methods should comply with the provisions of Class 2 products in GB6543. The net weight of each box of this product is 20kg or the specifications and dimensions of the packaging are determined according to user requirements. 6.2.2 Plastic woven bag and plastic bag packaging. The inner packaging adopts polyethylene plastic film bag, specification size: 800mm×500mm or 600mm×400mm, thickness of 0.08mm, and the outer packaging adopts plastic woven bag, specification size: 700mm×450mm or 500mm×350mm, and its performance and inspection method shall comply with the provisions of GB8946A. The net weight of each bag of this product is 50kg or 25kg. 6.3 Packaging procedure of trisodium chlorinated phosphate
6.3.1 Double corrugated carton and plastic bag packaging. The inner packaging plastic bag is tightly sealed with a heat sealer, and the outer packaging box is sealed with kraft paper or tape paper, with a width of 80~90mm, and the length must exceed the two ends of the carton and droop 50~60mm. 5
W.bzsosO.coI HG/T2528—93
6.3.2 Plastic textile bag and plastic bag packaging. The inner packaging plastic bag is tied manually with vinyl rope or rope of equivalent quality, or sealed with other equivalent methods. The outer bag is folded at a distance of not less than 30mm from the bag edge, and the edge is sewn with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the bag edge. The stitch length is 7-12mm, the stitches are neat and the stitch length is uniform. There are no leaks or skipped stitches. 6.4 Chlorotrisodium phosphate should be covered during transportation to prevent sun exposure, rain, and moisture. It should not be mixed with acidic substances. 6.5 Chlorotrisodium phosphate should be stored in a cool and dry place to prevent rain and moisture. Prevent sun exposure and heat. It should not be mixed with acidic substances. 6.6 Under the conditions of packaging, storage and transportation in accordance with this standard, the effective chlorine content loss rate of this product should not exceed 5% within 6 months from the date of leaving the factory.
Additional remarks:
This standard is 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 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 and Sichuan Chuanxi Phosphorus Chemical Industry Group Co., Ltd. The main drafters of this standard are Lu Siwei, Li Guangming, Liu Xiaoping, Li Difa and Liao Hongying. 6
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