Some standard content:
Chemical Industry Standard of the People's Republic of China
Water Treatment Agent
1 Subject Content and Scope of Application
Polyol Phosphate
HG 2228 -- 91
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation, storage and safety requirements for polyol phosphate products.
This standard applies to nitrogen-free polyol phosphates obtained by reacting glycerol polyoxyethylene ether with phosphorus pentoxide. It also applies to nitrogen-containing polyol phosphates obtained by reacting glycerol polyoxyethylene ether, ethanol, ethylene glycol ether and triethanolamine with phosphorus pentoxide. This product is mainly used as a scale inhibitor and corrosion inhibitor for industrial circulating cooling water treatment. Structural formula:
CH2 (CH2 --CH2—O)m
Wherein, RR. is H
n is 0,1
Referenced standards
GB 191
Packaging, storage and transportation diagrams
CH-(CH2--CH2-O)-, H
CH --(CH2--CH2 --O), H
CH--CH2--O-
CH2--CH2-O--H
CH2--CH2--OH
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagentsPreparation of preparations and products used in test methods for chemical reagentsGB603
General rules for sampling of chemical products
GB 6678
General rules for sampling of liquid chemical products
GB 6680
3 Product Classification
This product is divided into:
Class A: Polyol phosphate ester without nitrogen; approved by the Ministry of Chemical Industry of the People's Republic of China on November 15, 1991, 108
Implementation on July 1, 1992
Class B: Polyol phosphate ester containing nitrogen.
4 Technical Requirements
4.1 Appearance
HG 2228: 91
Class A is brown paste; Class B is brown viscous liquid. 4.2 Technical conditions
Polyol phosphates shall meet the requirements of Table 1:
Organic phosphate (as P(4) content, %
Inorganic phosphoric acid (as PO), %
PH chain (1% aqueous solution)
5 Test methods
Qualified products
Qualified products
Except for special provisions in the test methods, only analytical reagents and distilled water or water of equivalent purity shall be used, and the base material shall be a reference reagent.
Standard solutions and preparations required for determination shall be prepared in accordance with the provisions of GB601.GB603 unless otherwise specified. 5.1 Determination of organic phosphate and inorganic phosphoric acid content in Class A products 5.1.1 Summary of methods
Class A products contain organic phosphate (containing organic mono- and di-phosphoric acids) and unreacted phosphorus pentoxide (with aquatic or inorganic phosphoric acid), which can be titrated continuously by neutralization method. The first stoichiometric point is indicated by modified methyl orange, the second stoichiometric point is indicated by phenolic acid, and the third stoichiometric point is determined after adding calcium chloride for conversion. The content of organic phosphoric acid (the sum of the content of monoester and diester) and inorganic phosphoric acid is calculated from the amount of alkali solution consumed at each stoichiometric point. For ease of calculation, each component is calculated as phosphate (PO-). Reaction equation:
First stoichiometric point: R,HPO,+NaOH-R,NaPO+H2ORH,PO + NaOH - RNaHPO, +H,O
H,PO +NaOH -NaH,PO, +H2O
Second stoichiometric point: RNaHPO.+NaOH-RNa2PO+HONaH,PO, + NaOH-Na HPO +H,O
Third stoichiometric point: 2Na2HPO,+3CaCl2=Ca(PO)2→+2HCI+4NaCIH++OH-H,O
Where: R2HPO and RH2PO are organic phosphate diester and monoester, respectively. 5.1.2 Reagents and materials
5.1.2.1 Sodium hydroxide (GB629) standard solution: c(NaOH) 0.5 mol/l5.1.2.2 Sodium chloride (GB1266) saturated solution;5.1.2.3 Anhydrous calcium chloride (GB3208) saturated solution;5.1.2.4 Phenol (G110729) indicator: 10 g/LEthanol solution:5. 1. 2. 5
Methyl orange (HG3089) indicator: 2.0 g/LSolution: Dimethyl blue FF solution: 2.8 g/L;
HG 2228—91
5.1.2.7 Modified methyl orange indicator: Mix 5.1.2.5 and 5.1.2.6 in equal volumes. 5.1.3 Analysis steps
Weigh about 2.5g of sample in a weighing bottle, accurate to 0.0002g, dissolve it in water without carbon dioxide, and transfer the sample to a 250ml conical flask. Adjust the volume to 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and three drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.1.2.1). When the solution changes from purple to bright green, it is the stoichiometric point. The volume of standard solution consumed is V:
Add three drops of phenolic acid indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.1.2.1). When the solution turns slightly red within 30s, The first stoichiometric point is when it does not fade, and the volume of standard solution consumed is V2. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.1.2.1). When the solution turns slightly red and does not fade within 30 seconds, it is the third stoichiometric point, and the volume of standard solution consumed is V3. 5.1.4 Expression of analysis results
5.1.4.1 The organic phosphate content X, expressed as mass percentage (calculated as PO\), is calculated according to formula (1): X,X2+X3
Wherein: X, organic phosphate monoester content (calculated as PO-), %: obtained from formula (2); X-. Organic phosphate diester content (calculated as PO-), %; obtained from formula (3). The organic phosphate monoester X expressed as a mass percentage (in terms of PO-) is calculated according to formula (2): c(V2-Vs)X0. 095
wherein, V. The volume of sodium hydroxide standard solution consumed at the first stoichiometric point, mL, the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL: V
.·The actual concentration of the sodium hydroxide standard solution, mol(1)
The mass of the sample is calculated, 0.095-the mass of phosphate (PO3-) in grams equivalent to 1.00mL of sodium hydroxide standard solution (Lc (NaOH) = 1.000mol/L).
The result should be expressed to two decimal places.
Organic phosphate diester content X (in PO) expressed as a mass percentage. Calculated according to formula (3): c(VV,)×(0. 095) ×100
Wherein: Volume of sodium hydroxide standard solution consumed at the first stoichiometric point, mL.V. ... Volume of sodium hydroxide standard solution consumed at the second stoichiometric point, mL.·Actual concentration of sodium hydroxide standard solution, mol/L; (3)
…Mass of sample·C·
0.09Mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Ce (NaOH) 1.000mol/L3, expressed in grams.
The result should be expressed to two decimal places.
5.1.4.2 The content of inorganic phosphoric acid X (in PO-) expressed as a mass percentage shall be calculated according to formula (4): rV,X0.095
Wherein: The volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL. The actual concentration of sodium hydroxide standard solution, mol/L; (4)
mThe mass of the sample·g
The mass of phosphate 0.093-
(PO) expressed in grams equivalent to 1.00mL sodium hydroxide standard solution Cc (NaOH) 1,000mol/L)
The result shall be expressed to two decimal places.
5.1.5 Tolerance
HG 2228-91
Take the arithmetic mean of the results of two parallel determinations as the determination result. The absolute difference between the results of parallel determination of each component should not exceed: 0.30% for organic phosphoric acid; 0.30% for inorganic phosphoric acid.
The absolute difference between the results of determination of each component in different laboratories should not exceed: 0.50% for organic phosphoric acid; 0.60% for inorganic phosphoric acid. 5.2 Determination of pH value of Category A products
5.2.1 Instruments and equipment
5.2.1.1 Acidometer: the scale value is 0.02 pH unit, equipped with glass electrode and saturated calomel electrode. 5.2.2 Analysis steps
Weigh 1.00g of sample in a beaker, dissolve it with water, dilute it to 100ml with water, mix it evenly, immerse the calomel electrode and glass electrode in the sample to be tested, and measure the pH value of the sample on the positioned acidometer. The difference between the results of two parallel tests shall not exceed 0.2 pH unit. The arithmetic mean is taken as the determination result. 5.3 Determination of organic phosphate and inorganic phosphoric acid content in Category B products 5.3.1 Summary of method
Category B products contain organic phosphate (including nitrogen-free and nitrogen-containing phosphate) and unreacted phosphorus pentoxide (generating inorganic phosphoric acid with water). Except that isopropanol needs to be added before the second chemical measurement point to change the dielectric constant of the system, the rest is the same as 5.1.1. 5.3.2 Reagents and materials
5.3.2.1 Sodium hydroxide (GB629) standard solution: c(NaOH) 0.1mol/L5.3.2.2 Isopropanol (GB7814);
5.3.2.3 Neutral isopropanol: Add two drops of phenolic acid indicator (5.1.2.4) to (5.3.2.2) and neutralize with 0.1mol/1 sodium hydroxide solution (5.3.2.1) until the solution turns slightly red and does not fade within 30s. Prepare it when needed and store it in a brown bottle; 5.3.2.4 Other reagents are the same as 5.1.2.
5.3.3 Analysis steps
Weigh about 1.2g of the sample, accurate to 0.0002g, dissolve it in water without carbon dioxide, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and shake it well.
Take 25.00ml of the above test solution in a conical flask, adjust the volume to about 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and two drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution changes from purple to bright green, it is the first chemical bright spot. The consumed standard solution liquid is V. Add 20mL of neutral isopropanol (5.3.2.3) and three drops of phenol indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.3.2 .1) Titrate until the solution turns slightly red and does not fade within 30 seconds, which is the second chemical quantification point. The volume of standard solution consumed is V. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns slightly red and does not fade within 30 seconds, it is the third chemical quantification point. The volume of standard solution consumed is V3. 5.3.4 Expression of analytical results
5.3.4.1 The content of organic phosphate ester expressed as mass percentage (in terms of PO-) is calculated according to formula (5): X, a X+X,
Where: X. - The content of organic phosphate ester containing no nitrogen (in terms of PO), %, is obtained from formula (6); X, - The content of organic phosphate aldehyde containing nitrogen (in terms of PO~), %, is obtained from formula (7). The result should be expressed to two decimal places.
The content of organic phosphate ester containing no nitrogen expressed as mass percentage X. (in terms of PO), calculated according to formula (6): XV.,)x0.095 x1...
Wherein: V-the volume of sodium hydroxide standard solution consumed at the second stoichiometric point, mL; V.--the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL, (5)
(6)
XG2228-91
actual concentration of sodium hydroxide standard solution, mol/1; m the mass of the sample, g;
0.095--the mass of phosphate (PO) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/1) in grams.
The result should be expressed to two decimal places.
The nitrogen-containing organic phosphate content X, expressed as a mass percentage (in terms of PO), is calculated according to formula (7): X,-c(V.-Va)×0. 095 ×100-
Wherein; V. The volume of sodium hydroxide standard solution consumed at the stoichiometric point, mL; V.--·The volume of sodium hydroxide standard solution consumed at the stoichiometric point, ml; c-the actual concentration of sodium hydroxide standard solution mol/L; mThe mass of the sample, g;
0.095--The mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/LJ, expressed in grams.
The result should be expressed to two decimal places.
5.3.4.2 The inorganic phosphoric acid content X (in PO-) expressed as a mass percentage is calculated according to the formula (8): cV.×0.095×100
Wherein: V is the volume of the sodium hydroxide standard solution consumed at the third stoichiometric point, mL; c is the actual concentration of the sodium hydroxide standard solution, maol/L; (8)wwW.bzxz.Net
m is the mass of the sample, g;
0.095---the mass of phosphate (PO-) equivalent to 1.00mL of sodium hydroxide standard solution Cc (NaOH) 1.000mol/L3, expressed in grams.|| tt||The result should be expressed to two decimal places.
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results of each component shall not be greater than: 0.30% for organic phosphate ester: 0.30% for inorganic phosphoric acid.
The absolute difference of the determination results of each component in different laboratories shall not be greater than: 0.45% for organic phosphate ester, 0.60% for inorganic phosphoric acid. 5.4 Determination of pH value of Class B products
Same as 5.2.
6 Inspection and testing
6.1 Polyol phosphate products shall be tested by the manufacturer The quality inspection department shall inspect the product quality according to the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. 6.2 Each batch of products leaving the factory shall be accompanied by a quality certificate in a certain format, the contents of which shall include: manufacturer name, product name, production date, batch number, net weight, proof that the product quality meets this standard and the number of this standard. 6.3 The user unit has the right to conduct quality inspection on the received products according to the provisions of this standard to verify whether its quality meets the requirements of this standard. 6.4 The manufacturer shall inspect the products leaving the factory by batch, and the weight of each batch of products shall be 1 t. 6. 5 Determine the number of sampling units in accordance with Article 6.6 of GB6678. When sampling, insert a plastic tube into the barrel, stir evenly, and take out the sample at 5/6 of the depth of the barrel. The sample taken out from each barrel must not be less than 50g. Put the obtained samples into a clean, dry bottle and mix evenly. Take 100g from the uniform sample and put it in two clean, dry wide-mouth bottles with ground mouths. Seal the bottle mouths, attach labels, and indicate: product name, batch number, production date, sampling date and name of the sampler, etc. One bottle is inspected by the quality inspection department, and the other bottle is a reserved sample for re-inspection or arbitration. The retention period is six months
HG 2228--91
6.6 If any of the test results do not meet the requirements of this standard, in addition to re-testing the original sample, samples should be taken from the packaging container with twice the amount for re-testing. If there is still one item that does not meet the requirements of this standard, the entire batch of products will not be accepted. 6.7 When the supply and demand parties have disputes over product quality and need arbitration, they should be carried out in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 7 Marking, packaging, transportation and storage
7.1 There should be obvious solid marks on each package, including: manufacturer name, product name, trademark, grade, batch number, net weight, production date and number of this standard; and painted with moisture-proof and upward signs. 7.2 Polyol-free phosphate products are packaged in wide-mouth polyethylene barrels, with a net weight of 50kg per barrel. The barrel mouth is first sealed with an inner cap and then tightened with a threaded outer cap.
7.3 Polyol phosphoric acid can be transported by water, land and air transportation. During transportation, a awning should be provided, and collisions should be prevented during loading, unloading and transportation. 7.4 Polyol phosphates should be stored in a cool and dry place and must be isolated from acidic or alkaline chemicals during storage and transportation. The storage period is one year.
8 Safety requirements
During loading and unloading, operators should wear gloves to avoid direct contact. If any material escapes, it should be rinsed with a large amount of water, and the washing water should be discharged into the wastewater system after dilution. Additional notes:
This standard was proposed by the Science and Technology Office 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 Nanjing Chemical Engineering Design Institute. The main drafters of this standard are Lin Zhuxin, Chen Dingjin, and Lu Lang. 1132 Analysis steps
Weigh 1.00g of sample in a beaker, dissolve it in water, dilute it to 100ml with water, stir evenly, immerse the calomel electrode and glass electrode in the sample to be tested, and measure the pH value of the sample on the positioned acidometer. The difference between the results of two parallel tests shall not exceed 0.2pH units. Take the arithmetic mean as the test result. 5.3 Determination of organic phosphate and inorganic phosphoric acid content in Class B products 5.3.1 Method summary
Class B products contain organic phosphate (including nitrogen-free and nitrogen-containing phosphates) and unreacted phosphorus pentoxide (generating inorganic phosphoric acid with water). Except that isopropanol needs to be added before the second chemical measurement point to change the dielectric constant of the system, the rest is the same as 5.1.1. 5.3.2 Reagents and materials
5.3.2.1 Sodium hydroxide (GB629) standard solution: c(NaOH) 0.1mol/L5.3.2.2 Isopropanol (GB7814);
5.3.2.3 Neutral isopropanol: Add two drops of phenolic acid indicator (5.1.2.4) to (5.3.2.2) and neutralize with 0.1mol/1 sodium hydroxide solution (5.3.2.1) until the solution turns slightly red and does not fade within 30s. Prepare it before use and store it in a brown bottle; 5.3.2.4 Other reagents are the same as in 5.1.2.
5.3.3 Analysis steps
Weigh about 1.2g of sample, accurate to 0.0002g, dissolve it in water without carbon dioxide, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and shake it well.
Take 25.00ml of the above test solution in a conical flask, adjust the volume to about 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and two drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns from purple to bright green, it is the first chemical bright spot. The amount of standard solution consumed is V. Add 20mL of neutral isopropanol (5.3.2.3) and three drops of phenol indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.3.2.1). .1) Titrate until the solution turns slightly red and does not fade within 30 seconds, which is the second chemical quantification point. The volume of standard solution consumed is V. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns slightly red and does not fade within 30 seconds, it is the third chemical quantification point. The volume of standard solution consumed is V3. 5.3.4 Expression of analytical results
5.3.4.1 The content of organic phosphate ester expressed as mass percentage (in terms of PO-) is calculated according to formula (5): X, a X+X,
Where: X. - The content of organic phosphate ester containing no nitrogen (in terms of PO), %, is obtained from formula (6); X, - The content of organic phosphate aldehyde containing nitrogen (in terms of PO~), %, is obtained from formula (7). The result should be expressed to two decimal places.
The content of organic phosphate ester containing no nitrogen expressed as mass percentage X. (in terms of PO), calculated according to formula (6): XV.,)x0.095 x1...
Wherein: V-the volume of sodium hydroxide standard solution consumed at the second stoichiometric point, mL; V.--the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL, (5)
(6)
XG2228-91
actual concentration of sodium hydroxide standard solution, mol/1; m the mass of the sample, g;
0.095--the mass of phosphate (PO) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/1) in grams.
The result should be expressed to two decimal places.
The nitrogen-containing organic phosphate content X, expressed as a mass percentage (in terms of PO), is calculated according to formula (7): X,-c(V.-Va)×0. 095 ×100-
Wherein; V. The volume of sodium hydroxide standard solution consumed at the stoichiometric point, mL; V.--·The volume of sodium hydroxide standard solution consumed at the stoichiometric point, ml; c-The actual concentration of sodium hydroxide standard solution mol/L; mThe mass of the sample, g;
0.095--The mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/LJ, expressed in grams.
The result should be expressed to two decimal places.
5.3.4.2 The inorganic phosphoric acid content X (in PO-) expressed as a mass percentage is calculated according to the formula (8): cV.×0.095×100
Wherein: V is the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL; c is the actual concentration of sodium hydroxide standard solution, maol/L; (8)
m is the mass of the sample, g;
0.095---the mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Cc (NaOH) 1.000mol/L3, expressed in grams.|| tt||The result should be expressed to two decimal places.
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results of each component shall not be greater than: 0.30% for organic phosphate ester: 0.30% for inorganic phosphoric acid.
The absolute difference of the determination results of each component in different laboratories shall not be greater than: 0.45% for organic phosphate ester, 0.60% for inorganic phosphoric acid. 5.4 Determination of pH value of Class B products
Same as 5.2.
6 Inspection and testing
6.1 Polyol phosphate products shall be tested by the manufacturer The quality inspection department shall inspect the product quality according to the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. 6.2 Each batch of products leaving the factory shall be accompanied by a quality certificate in a certain format, the contents of which shall include: manufacturer name, product name, production date, batch number, net weight, proof that the product quality meets this standard and the number of this standard. 6.3 The user unit has the right to conduct quality inspection on the received products according to the provisions of this standard to verify whether its quality meets the requirements of this standard. 6.4 The manufacturer shall inspect the products leaving the factory by batch, and the weight of each batch of products shall be 1 t. 6. 5 Determine the number of sampling units in accordance with Article 6.6 of GB6678. When sampling, insert a plastic tube into the barrel, stir evenly, and take out the sample at 5/6 of the depth of the barrel. The sample taken out from each barrel must not be less than 50g. Put the obtained samples into a clean, dry bottle and mix them evenly. Take 100g from the uniform sample and put it in two clean, dry wide-mouth bottles with ground mouths. Seal the bottle mouths, attach labels, and indicate: product name, batch number, production date, sampling date and name of the sampler, etc. One bottle is inspected by the quality inspection department, and the other bottle is a reserved sample for re-inspection or arbitration. The retention period is six months
HG 2228--91
6.6 If any of the test results do not meet the requirements of this standard, in addition to re-testing the original sample, samples should be taken from the packaging container with twice the amount for re-testing. If there is still one item that does not meet the requirements of this standard, the entire batch of products will not be accepted. 6.7 When the supply and demand parties have disputes over product quality and need arbitration, they should be carried out in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 7 Marking, packaging, transportation and storage
7.1 There should be obvious solid marks on each package, including: manufacturer name, product name, trademark, grade, batch number, net weight, production date and number of this standard; and painted with moisture-proof and upward signs. 7.2 Polyol-free phosphate products are packaged in wide-mouth polyethylene barrels, with a net weight of 50kg per barrel. The barrel mouth is first sealed with an inner cap and then tightened with a threaded outer cap.
7.3 Polyol phosphoric acid can be transported by water, land and air transportation. During transportation, a awning should be provided, and collisions should be prevented during loading, unloading and transportation. 7.4 Polyol phosphates should be stored in a cool and dry place and must be isolated from acidic or alkaline chemicals during storage and transportation. The storage period is one year.
8 Safety requirements
During loading and unloading, operators should wear gloves to avoid direct contact. If any material escapes, it should be rinsed with a large amount of water, and the washing water should be discharged into the wastewater system after dilution. Additional remarks:
This standard was proposed by the Science and Technology Office 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 Nanjing Chemical Engineering Design Institute. The main drafters of this standard are Lin Zhuxin, Chen Dingjin, and Lu Lang. 1132 Analysis steps
Weigh 1.00g of sample in a beaker, dissolve it in water, dilute it to 100ml with water, stir evenly, immerse the calomel electrode and glass electrode in the sample to be tested, and measure the pH value of the sample on the positioned acidometer. The difference between the results of two parallel tests shall not exceed 0.2pH units. Take the arithmetic mean as the test result. 5.3 Determination of organic phosphate and inorganic phosphoric acid content in Class B products 5.3.1 Method summary
Class B products contain organic phosphate (including nitrogen-free and nitrogen-containing phosphates) and unreacted phosphorus pentoxide (generating inorganic phosphoric acid with water). Except that isopropanol needs to be added before the second chemical measurement point to change the dielectric constant of the system, the rest is the same as 5.1.1. 5.3.2 Reagents and materials
5.3.2.1 Sodium hydroxide (GB629) standard solution: c(NaOH) 0.1mol/L5.3.2.2 Isopropanol (GB7814);
5.3.2.3 Neutral isopropanol: Add two drops of phenolic acid indicator (5.1.2.4) to (5.3.2.2) and neutralize with 0.1mol/1 sodium hydroxide solution (5.3.2.1) until the solution turns slightly red and does not fade within 30s. Prepare it before use and store it in a brown bottle; 5.3.2.4 Other reagents are the same as in 5.1.2.
5.3.3 Analysis steps
Weigh about 1.2g of sample, accurate to 0.0002g, dissolve it in water without carbon dioxide, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and shake it well.
Take 25.00ml of the above test solution in a conical flask, adjust the volume to about 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and two drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns from purple to bright green, it is the first chemical bright spot. The amount of standard solution consumed is V. Add 20mL of neutral isopropanol (5.3.2.3) and three drops of phenol indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.3.2.1). .1) Titrate until the solution turns slightly red and does not fade within 30 seconds, which is the second chemical quantification point. The volume of standard solution consumed is V. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns slightly red and does not fade within 30 seconds, it is the third chemical quantification point. The volume of standard solution consumed is V3. 5.3.4 Expression of analytical results
5.3.4.1 The content of organic phosphate ester expressed as mass percentage (in terms of PO-) is calculated according to formula (5): X, a X+X,
Where: X. - The content of organic phosphate ester containing no nitrogen (in terms of PO), %, is obtained from formula (6); X, - The content of organic phosphate aldehyde containing nitrogen (in terms of PO~), %, is obtained from formula (7). The result should be expressed to two decimal places.
The content of organic phosphate ester containing no nitrogen expressed as mass percentage X. (in terms of PO), calculated according to formula (6): XV.,)x0.095 x1...
Wherein: V-the volume of sodium hydroxide standard solution consumed at the second stoichiometric point, mL; V.--the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL, (5)
(6)
XG2228-91
actual concentration of sodium hydroxide standard solution, mol/1; m the mass of the sample, g;
0.095--the mass of phosphate (PO) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/1) in grams.
The result should be expressed to two decimal places.
The nitrogen-containing organic phosphate content X, expressed as a mass percentage (in terms of PO), is calculated according to formula (7): X,-c(V.-Va)×0. 095 ×100-
Wherein; V. The volume of sodium hydroxide standard solution consumed at the stoichiometric point, mL; V.--·The volume of sodium hydroxide standard solution consumed at the stoichiometric point, ml; c-the actual concentration of sodium hydroxide standard solution mol/L; mThe mass of the sample, g;
0.095--The mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/LJ, expressed in grams.
The result should be expressed to two decimal places.
5.3.4.2 The inorganic phosphoric acid content X (in PO-) expressed as a mass percentage is calculated according to the formula (8): cV.×0.095×100
Wherein: V is the volume of the sodium hydroxide standard solution consumed at the third stoichiometric point, mL; c is the actual concentration of the sodium hydroxide standard solution, maol/L; (8)
m is the mass of the sample, g;
0.095---the mass of phosphate (PO-) equivalent to 1.00mL of sodium hydroxide standard solution Cc (NaOH) 1.000mol/L3, expressed in grams.|| tt||The result should be expressed to two decimal places.
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results of each component shall not be greater than: 0.30% for organic phosphate ester: 0.30% for inorganic phosphoric acid.
The absolute difference of the determination results of each component in different laboratories shall not be greater than: 0.45% for organic phosphate ester, 0.60% for inorganic phosphoric acid. 5.4 Determination of pH value of Class B products
Same as 5.2.
6 Inspection and testing
6.1 Polyol phosphate products shall be tested by the manufacturer The quality inspection department shall inspect the product quality according to the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. 6.2 Each batch of products leaving the factory shall be accompanied by a quality certificate in a certain format, the contents of which shall include: manufacturer name, product name, production date, batch number, net weight, proof that the product quality meets this standard and the number of this standard. 6.3 The user unit has the right to conduct quality inspection on the received products according to the provisions of this standard to verify whether its quality meets the requirements of this standard. 6.4 The manufacturer shall inspect the products leaving the factory by batch, and the weight of each batch of products shall be 1 t. 6. 5 Determine the number of sampling units in accordance with Article 6.6 of GB6678. When sampling, insert a plastic tube into the barrel, stir evenly, and take out the sample at 5/6 of the depth of the barrel. The sample taken out from each barrel must not be less than 50g. Put the obtained samples into a clean, dry bottle and mix evenly. Take 100g from the uniform sample and put it in two clean, dry wide-mouth bottles with ground mouths. Seal the bottle mouths, attach labels, and indicate: product name, batch number, production date, sampling date and name of the sampler, etc. One bottle is inspected by the quality inspection department, and the other bottle is a reserved sample for re-inspection or arbitration. The retention period is six months
HG 2228--91
6.6 If any of the test results do not meet the requirements of this standard, in addition to re-testing the original sample, samples should be taken from the packaging container with twice the amount for re-testing. If there is still one item that does not meet the requirements of this standard, the entire batch of products will not be accepted. 6.7 When the supply and demand parties have disputes over product quality and need arbitration, they should be carried out in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 7 Marking, packaging, transportation and storage
7.1 There should be obvious solid marks on each package, including: manufacturer name, product name, trademark, grade, batch number, net weight, production date and number of this standard; and painted with moisture-proof and upward signs. 7.2 Polyol-free phosphate products are packaged in wide-mouth polyethylene barrels, with a net weight of 50kg per barrel. The barrel mouth is first sealed with an inner cap and then tightened with a threaded outer cap.
7.3 Polyol phosphoric acid can be transported by water, land and air transportation. During transportation, a awning should be provided, and collisions should be prevented during loading, unloading and transportation. 7.4 Polyol phosphates should be stored in a cool and dry place and must be isolated from acidic or alkaline chemicals during storage and transportation. The storage period is one year.
8 Safety requirements
During loading and unloading, operators should wear gloves to avoid direct contact. If any material escapes, it should be rinsed with a large amount of water, and the washing water should be discharged into the wastewater system after dilution. Additional remarks:
This standard was proposed by the Science and Technology Office 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 Nanjing Chemical Engineering Design Institute. The main drafters of this standard are Lin Zhuxin, Chen Dingjin, and Lu Lang. 1131 Method Summary
Products in category B contain organic phosphates (including nitrogen-free and nitrogen-containing phosphates) and unreacted phosphorus pentoxide (which reacts with water to form inorganic phosphoric acid). Except that isopropanol needs to be added before the second stoichiometric point to change the dielectric constant of the system, the rest is the same as in 5.1.1. 5.3.2 Reagents and Materials
5.3.2.1 Sodium hydroxide (GB629) standard solution: c(NaOH) 0.1mol/L5.3.2.2 Isopropanol (GB7814);
5.3.2.3 Neutral isopropanol: Add two drops of phenolic acid indicator (5.1.2.4) to (5.3.2.2) and neutralize with 0.1mol/1 sodium hydroxide solution (5.3.2.1) until the solution turns slightly red and does not fade within 30s. Prepare immediately before use and store in a brown bottle; 5.3.2.4 Other reagents are the same as 5.1.2.
5.3.3 Analysis steps
Weigh about 1.2g of sample, accurate to 0.0002g, dissolve it in water without carbon dioxide, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and shake well.
Take 25.00ml of the above test solution in a conical flask, adjust the volume to about 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and two drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution changes from purple to bright green, it is the first chemical point. The amount of standard solution consumed is V. Add 20mL of neutral isopropanol (5.3.2.3) and three drops of phenol indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.3.2 .1) Titrate until the solution turns slightly red and does not fade within 30 seconds, which is the second chemical quantification point. The volume of standard solution consumed is V. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns slightly red and does not fade within 30 seconds, it is the third chemical quantification point. The volume of standard solution consumed is V3. 5.3.4 Expression of analytical results
5.3.4.1 The content of organic phosphate ester expressed as mass percentage (in terms of PO-) is calculated according to formula (5): X, a X+X,
Where: X. - The content of organic phosphate ester containing no nitrogen (in terms of PO), %, is obtained from formula (6); X, - The content of organic phosphate aldehyde containing nitrogen (in terms of PO~), %, is obtained from formula (7). The result should be expressed to two decimal places.
The content of organic phosphate ester containing no nitrogen expressed as mass percentage X. (in terms of PO), calculated according to formula (6): XV.,)x0.095 x1...
Wherein: V-the volume of sodium hydroxide standard solution consumed at the second stoichiometric point, mL; V.--the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL, (5)
(6)
XG2228-91
actual concentration of sodium hydroxide standard solution, mol/1; m the mass of the sample, g;
0.095--the mass of phosphate (PO) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/1) in grams.
The result should be expressed to two decimal places.
The nitrogen-containing organic phosphate content X, expressed as a mass percentage (in terms of PO), is calculated according to formula (7): X,-c(V.-Va)×0. 095 ×100-
Wherein; V. The volume of sodium hydroxide standard solution consumed at the stoichiometric point, mL; V.--·The volume of sodium hydroxide standard solution consumed at the stoichiometric point, ml; c-the actual concentration of sodium hydroxide standard solution mol/L; mThe mass of the sample, g;
0.095--The mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/LJ, expressed in grams.
The result should be expressed to two decimal places.
5.3.4.2 The inorganic phosphoric acid content X (in PO-) expressed as a mass percentage is calculated according to the formula (8): cV.×0.095×100
Wherein: V is the volume of the sodium hydroxide standard solution consumed at the third stoichiometric point, mL; c is the actual concentration of the sodium hydroxide standard solution, maol/L; (8)
m is the mass of the sample, g;
0.095---the mass of phosphate (PO-) equivalent to 1.00mL of sodium hydroxide standard solution Cc (NaOH) 1.000mol/L3, expressed in grams.|| tt||The result should be expressed to two decimal places.
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results of each component shall not be greater than: 0.30% for organic phosphate ester: 0.30% for inorganic phosphoric acid.
The absolute difference of the determination results of each component in different laboratories shall not be greater than: 0.45% for organic phosphate ester, 0.60% for inorganic phosphoric acid. 5.4 Determination of pH value of Class B products
Same as 5.2.
6 Inspection and testing
6.1 Polyol phosphate products shall be tested by the manufacturer The quality inspection department shall inspect the product quality according to the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. 6.2 Each batch of products leaving the factory shall be accompanied by a quality certificate in a certain format, the contents of which shall include: manufacturer name, product name, production date, batch number, net weight, proof that the product quality meets this standard and the number of this standard. 6.3 The user unit has the right to conduct quality inspection on the received products according to the provisions of this standard to verify whether its quality meets the requirements of this standard. 6.4 The manufacturer shall inspect the products leaving the factory by batch, and the weight of each batch of products shall be 1 t. 6. 5 Determine the number of sampling units in accordance with Article 6.6 of GB6678. When sampling, insert a plastic tube into the barrel, stir evenly, and take out the sample at 5/6 of the depth of the barrel. The sample taken out from each barrel must not be less than 50g. Put the obtained samples into a clean, dry bottle and mix them evenly. Take 100g from the uniform sample and put it in two clean, dry wide-mouth bottles with ground mouths. Seal the bottle mouths, attach labels, and indicate: product name, batch number, production date, sampling date and name of the sampler, etc. One bottle is inspected by the quality inspection department, and the other bottle is a reserved sample for re-inspection or arbitration. The retention period is six months
HG 2228--91
6.6 If any of the test results do not meet the requirements of this standard, in addition to re-testing the original sample, samples should be taken from the packaging container with twice the amount for re-testing. If there is still one item that does not meet the requirements of this standard, the entire batch of products will not be accepted. 6.7 When the supply and demand parties have disputes over product quality and need arbitration, they should be carried out in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 7 Marking, packaging, transportation and storage
7.1 There should be obvious solid marks on each package, including: manufacturer name, product name, trademark, grade, batch number, net weight, production date and number of this standard; and painted with moisture-proof and upward signs. 7.2 Polyol-free phosphate products are packaged in wide-mouth polyethylene barrels, with a net weight of 50kg per barrel. The barrel mouth is first sealed with an inner cap and then tightened with a threaded outer cap.
7.3 Polyol phosphoric acid can be transported by water, land and air transportation. During transportation, a awning should be provided, and collisions should be prevented during loading, unloading and transportation. 7.4 Polyol phosphates should be stored in a cool and dry place and must be isolated from acidic or alkaline chemicals during storage and transportation. The storage period is one year.
8 Safety requirements
During loading and unloading, operators should wear gloves to avoid direct contact. If any material escapes, it should be rinsed with a large amount of water, and the washing water should be discharged into the wastewater system after dilution. Additional notes:
This standard was proposed by the Science and Technology Office 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 Nanjing Chemical Engineering Design Institute. The main drafters of this standard are Lin Zhuxin, Chen Dingjin, and Lu Lang. 1131 Method Summary
Products in category B contain organic phosphates (including nitrogen-free and nitrogen-containing phosphates) and unreacted phosphorus pentoxide (which reacts with water to form inorganic phosphoric acid). Except that isopropanol needs to be added before the second stoichiometric point to change the dielectric constant of the system, the rest is the same as in 5.1.1. 5.3.2 Reagents and Materials
5.3.2.1 Sodium hydroxide (GB629) standard solution: c(NaOH) 0.1mol/L5.3.2.2 Isopropanol (GB7814);
5.3.2.3 Neutral isopropanol: Add two drops of phenolic acid indicator (5.1.2.4) to (5.3.2.2) and neutralize with 0.1mol/1 sodium hydroxide solution (5.3.2.1) until the solution turns slightly red and does not fade within 30s. Prepare immediately before use and store in a brown bottle; 5.3.2.4 Other reagents are the same as 5.1.2.
5.3.3 Analysis steps
Weigh about 1.2g of sample, accurate to 0.0002g, dissolve it in water without carbon dioxide, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and shake well.
Take 25.00ml of the above test solution in a conical flask, adjust the volume to about 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and two drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution changes from purple to bright green, it is the first chemical point. The amount of standard solution consumed is V. Add 20mL of neutral isopropanol (5.3.2.3) and three drops of phenol indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.3.2 .1) Titrate until the solution turns slightly red and does not fade within 30 seconds, which is the second chemical quantification point. The volume of standard solution consumed is V. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns slightly red and does not fade within 30 seconds, it is the third chemical quantification point. The volume of standard solution consumed is V3. 5.3.4 Expression of analytical results
5.3.4.1 The content of organic phosphate ester expressed as mass percentage (in terms of PO-) is calculated according to formula (5): X, a X+X,
Where: X. - The content of organic phosphate ester containing no nitrogen (in terms of PO), %, is obtained from formula (6); X, - The content of organic phosphate aldehyde containing nitrogen (in terms of PO~), %, is obtained from formula (7). The result should be expressed to two decimal places.
The content of organic phosphate ester containing no nitrogen expressed as mass percentage X. (in terms of PO), calculated according to formula (6): XV.,)x0.095 x1...
Wherein: V-the volume of sodium hydroxide standard solution consumed at the second stoichiometric point, mL; V.--the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL, (5)
(6)
XG2228-91
actual concentration of sodium hydroxide standard solution, mol/1; m the mass of the sample, g;
0.095--the mass of phosphate (PO) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/1) in grams.
The result should be expressed to two decimal places.
The nitrogen-containing organic phosphate content X, expressed as a mass percentage (in terms of PO), is calculated according to formula (7): X,-c(V.-Va)×0. 095 ×100-
Wherein; V. The volume of sodium hydroxide standard solution consumed at the stoichiometric point, mL; V.--·The volume of sodium hydroxide standard solution consumed at the stoichiometric point, ml; c-the actual concentration of sodium hydroxide standard solution mol/L; mThe mass of the sample, g;
0.095--The mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/LJ, expressed in grams.
The result should be expressed to two decimal places.
5.3.4.2 The inorganic phosphoric acid content X (in PO-) expressed as a mass percentage is calculated according to the formula (8): cV.×0.095×100
Wherein: V is the volume of the sodium hydroxide standard solution consumed at the third stoichiometric point, mL; c is the actual concentration of the sodium hydroxide standard solution, maol/L; (8)
m is the mass of the sample, g;
0.095---the mass of phosphate (PO-) equivalent to 1.00mL of sodium hydroxide standard solution Cc (NaOH) 1.000mol/L3, expressed in grams.|| tt||The result should be expressed to two decimal places.
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results of each component shall not be greater than: 0.30% for organic phosphate ester: 0.30% for inorganic phosphoric acid.
The absolute difference of the determination results of each component in different laboratories shall not be greater than: 0.45% for organic phosphate ester, 0.60% for inorganic phosphoric acid. 5.4 Determination of pH value of Class B products
Same as 5.2.
6 Inspection and testing
6.1 Polyol phosphate products shall be tested by the manufacturer The quality inspection department shall inspect the product quality according to the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. 6.2 Each batch of products leaving the factory shall be accompanied by a quality certificate in a certain format, the contents of which shall include: manufacturer name, product name, production date, batch number, net weight, proof that the product quality meets this standard and the number of this standard. 6.3 The user unit has the right to conduct quality inspection on the received products according to the provisions of this standard to verify whether its quality meets the requirements of this standard. 6.4 The manufacturer shall inspect the products leaving the factory by batch, and the weight of each batch of products shall be 1 t. 6. 5 Determine the number of sampling units in accordance with Article 6.6 of GB6678. When sampling, insert a plastic tube into the barrel, stir evenly, and take out the sample at 5/6 of the depth of the barrel. The sample taken out from each barrel must not be less than 50g. Put the obtained samples into a clean, dry bottle and mix evenly. Take 100g from the uniform sample and put it in two clean, dry wide-mouth bottles with ground mouths. Seal the bottle mouths, attach labels, and indicate: product name, batch number, production date, sampling date and name of the sampler, etc. One bottle is inspected by the quality inspection department, and the other bottle is a reserved sample for re-inspection or arbitration. The retention period is six months
HG 2228--91
6.6 If any of the test results do not meet the requirements of this standard, in addition to re-testing the original sample, samples should be taken from the packaging container with twice the amount for re-testing. If there is still one item that does not meet the requirements of this standard, the entire batch of products will not be accepted. 6.7 When the supply and demand parties have disputes over product quality and need arbitration, they should be carried out in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 7 Marking, packaging, transportation and storage
7.1 There should be obvious solid marks on each package, including: manufacturer name, product name, trademark, grade, batch number, net weight, production date and number of this standard; and painted with moisture-proof and upward signs. 7.2 Polyol-free phosphate products are packaged in wide-mouth polyethylene barrels, with a net weight of 50kg per barrel. The barrel mouth is first sealed with an inner cap and then tightened with a threaded outer cap.
7.3 Polyol phosphoric acid can be transported by water, land and air transportation. During transportation, a awning should be provided, and collisions should be prevented during loading, unloading and transportation. 7.4 Polyol phosphates should be stored in a cool and dry place and must be isolated from acidic or alkaline chemicals during storage and transportation. The storage period is one year.
8 Safety requirements
During loading and unloading, operators should wear gloves to avoid direct contact. If any material escapes, it should be rinsed with a large amount of water, and the washing water should be discharged into the wastewater system after dilution. Additional remarks:
This standard was proposed by the Science and Technology Office 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 Nanjing Chemical Engineering Design Institute. The main drafters of this standard are Lin Zhuxin, Chen Dingjin, and Lu Lang. 1133 Analysis steps
Weigh about 1.2g of the sample, accurate to 0.0002g, dissolve it in water without carbon dioxide, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and shake it well.
Take 25.00ml of the above test solution in a conical flask, adjust the volume to about 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and two drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution changes from purple to bright green, it is the first chemical point. The consumed standard solution liquid is V. Add 20mL of neutral isopropanol (5.3.2.3) and three drops of phenol indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.3.2 .1) Titrate until the solution turns slightly red and does not fade within 30 seconds, which is the second chemical quantification point. The volume of standard solution consumed is V. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution turns slightly red and does not fade within 30 seconds, it is the third chemical quantification point. The volume of standard solution consumed is V3. 5.3.4 Expression of analytical results
5.3.4.1 The content of organic phosphate ester expressed as mass percentage (in terms of PO-) is calculated according to formula (5): X, a X+X,
Where: X. - The content of organic phosphate ester containing no nitrogen (in terms of PO), %, is obtained from formula (6); X, - The content of organic phosphate aldehyde containing nitrogen (in terms of PO~), %, is obtained from formula (7). The result should be expressed to two decimal places.
The content of organic phosphate ester containing no nitrogen expressed as mass percentage X. (in terms of PO), calculated according to formula (6): XV.,)x0.095 x1...
Wherein: V-the volume of sodium hydroxide standard solution consumed at the second stoichiometric point, mL; V.--the volume of sodium hydroxide standard solution consumed at the third stoichiometric point, mL, (5)
(6)
XG2228-91
actual concentration of sodium hydroxide standard solution, mol/1; m the mass of the sample, g;
0.095--the mass of phosphate (PO) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/1) in grams.
The result should be expressed to two decimal places.
The nitrogen-containing organic phosphate content X, expressed as a mass percentage (in terms of PO), is calculated according to formula (7): X,-c(V.-Va)×0. 095 ×100-
Wherein; V. The volume of sodium hydroxide standard solution consumed at the stoichiometric point, mL; V.--·The volume of sodium hydroxide standard solution consumed at the stoichiometric point, ml; c-the actual concentration of sodium hydroxide standard solution mol/L; mThe mass of the sample, g;
0.095--The mass of phosphate (PO-) equivalent to 1.00mL sodium hydroxide standard solution Lc (NaOH) = 1.000mol/LJ, expressed in grams.
The result should be expressed to two decimal places.
5.3.4.2 The inorganic phosphoric acid content X (in PO-) expressed as a mass percentage is calculated according to the formula (8): cV.×0.095×100
Wherein: V is the volume of the sodium hydroxide standard solution consumed at the third stoichiometric point, mL; c is the actual concentration of the sodium hydroxide standard solution, maol/L; (8)
m is the mass of the sample, g;
0.095---the mass of phosphate (PO-) equivalent to 1.00mL of sodium hydroxide standard solution Cc (NaOH) 1.000mol/L3, expressed in grams.|| tt||The result should be expressed to two decimal places.
5.3.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results of each component shall not be greater than: 0.30% for organic phosphate ester: 0.30% for inorganic phosphoric acid.
The absolute difference of the determination results of each component in different laboratories shall not be greater than: 0.45% for organic phosphate ester, 0.60% for inorganic phosphoric acid. 5.4 Determination of pH value of Class B products
Same as 5.2.
6 Inspection and testing
6.1 Polyol phosphate products shall be tested by the manufacturer The quality inspection department shall inspect the product quality according to the test methods and inspection rules specified in this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. 6.2 Each batch of products leaving the factory shall be accompanied by a quality certificate in a certain format, the contents of which shall include: manufacturer name, product name, production date, batch number, net weight, proof that the product quality meets this standard and the number of this standard. 6.3 The user unit has the right to conduct quality inspection on the received products according to the provisions of this standard to verify whether its quality meets the requirements of this standard. 6.4 The manufacturer shall inspect the products leaving the factory by batch, and the weight of each batch of products shall be 1 t. 6. 5 Determine the number of sampling units in accordance with Article 6.6 of GB6678. When sampling, insert a plastic tube into the barrel, stir evenly, and take out the sample at 5/6 of the depth of the barrel. The sample taken out from each barrel must not be less than 50g. Put the obtained samples into a clean, dry bottle and mix evenly. Take 100g from the uniform sample and put it in two clean, dry wide-mouth bottles with ground mouths. Seal the bottle mouths, attach labels, and indicate: product name, batch number, production date, sampling date and name of the sampler, etc. One bottle is inspected by the quality inspection department, and the other bottle is a reserved sample for re-inspection or arbitration. The retention period is six months
HG 2228--91
6.6 If any of the test results do not meet the requirements of this standard, in addition to re-testing the original sample, samples should be taken from the packaging container with twice the amount for re-testing. If there is still one item that does not meet the requirements of this standard, the entire batch of products will not be accepted. 6.7 When the supply and demand parties have disputes over product quality and need arbitration, they should be carried out in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 7 Marking, packaging, transportation and storage
7.1 There should be obvious solid marks on each package, including: manufacturer name, product name, trademark, grade, batch number, net weight, production date and number of this standard; and painted with moisture-proof and upward signs. 7.2 Polyol-free phosphate products are packaged in wide-mouth polyethylene barrels, with a net weight of 50kg per barrel. The barrel mouth is first sealed with an inner cap and then tightened with a threaded outer cap.
7.3 Polyol phosphoric acid can be transported by water, land and air transportation. During transportation, a awning should be provided, and collisions should be prevented during loading, unloading and transportation. 7.4 Polyol phosphates should be stored in a cool and dry place and must be isolated from acidic or alkaline chemicals during storage and transportation. The storage period is one year.
8 Safety requirements
During loading and unloading, operators should wear gloves to avoid direct contact. If any material escapes, it should be rinsed with a large amount of water, and the washing water should be discharged into the wastewater system after dilution. Additional remarks:
This standard was proposed by the Science and Technology Office 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 Nanjing Chemical Engineering Design Institute. The main drafters of this standard are Lin Zhuxin, Chen Dingjin, and Lu Lang. 1133 Analysis steps
Weigh about 1.2g of the sample, accurate to 0.0002g, dissolve it in water without carbon dioxide, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and shake it well.
Take 25.00ml of the above test solution in a conical flask, adjust the volume to about 50mL with water, add 10mL of sodium chloride solution (5.1.2.2) and two drops of modified methyl orange indicator (5.1.2.7), and titrate with sodium hydroxide standard solution (5.3.2.1). When the solution changes from purple to bright green, it is the first chemical point. The consumed standard solution liquid is V. Add 20mL of neutral isopropanol (5.3.2.3) and three drops of phenol indicator (5.1.2.4) to the above solution, and titrate with sodium hydroxide standard solution (5.3.2 .1) Titrate until the solution turns slightly red and does not fade within 30 seconds, which is the second chemical quantification point. The volume of standard solution consumed is V. Add 5 mL of calcium chloride solution (5.1.2.3) to the above solution and titrate with sodium hydroxide standard solution (5.3.
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.