Some standard content:
HG/T3657—1999
Water treatment agent isothiazolinone derivative is a low-toxic, broad-spectrum, non-oxidizing biocide. Its active ingredients include 5-chloro-2-methyl-4-isothiazoline-3-one and 2-methyl-4-isothiazoline-3-one. This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Water Treatment Agent Branch of the National Technical Committee for Chemical Standardization. The main drafting units of this standard are: Shanghai Future Enterprise Co., Ltd., Beijing Changhua Fine Chemical Factory of the Chinese People's Liberation Army Chemical Defense Research Institute. The participating drafting units of this standard are: Inner Mongolia Bailing Fine Chemical Co., Ltd., and the main drafters of this standard are: Liu Xin, Zou Biyou, Zhou Gengyuan, Tao Weisheng, and Gao Ziyu. 213
1 Scope
Chemical Industry Standard of the People's Republic of China
Water treatment chemicals
Isothiazolinone derivatives
Water treatment chemicals-Isothiazolinones HG/T 3657.-- 1999
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation, storage and safety requirements for isothiazolinone derivatives of water treatment agents.
This product is mainly used as a biocide in industrial water treatment. The water treatment agent isothiazolinone derivatives mainly contain two components: a) 5-chloro-2-methyl-4-isothiazolin-3-one (CMI) Structural formula:
Relative molecular mass: 149.60 (according to the 1995 international relative atomic mass) b) 2-methyl-4-isothiazolin-3-one (MI) Structural formula:
Relative molecular mass: 115.16 (according to the 1995 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. Pictorial signs for packaging, storage and transportation
GB 191—19901
GB/T601·-1988 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T603—1988 Preparation of preparations and products used in test methods of chemical reagents (neqISO6353-1:1982)GR/T 1250--1989
GB/T 6678--1986
GH/T 6682--1992wwW.bzxz.Net
3 Product classification
This product is divided into two categories.
Methods for expressing and determining limit values General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories (neq1S0) 3696: 1986) Category 1: active matter content is 14%. Used to prepare products with an active matter content of 1.5%; Category 2: active matter content is 1.5%, used as a biocide. Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999 214
Implementation on June 1, 2000
4 Requirements
HG/T3657-1999
4.1 Appearance: Category 1 products are brown-yellow transparent liquids, and Category 2 products are light yellow or light green transparent liquids. 4.2 Water treatment agent isothiophenone derivatives shall meet the requirements of Table 1. Table 1
Active matter content, must
CM1/M1 (mass percentage)
Density (20 () + #/em*
5 Test method
1, 30
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and grade 3 water specified in GB/T6682. The standard solutions, preparations and products required in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601 and GB/T603. 5.1 Determination of active matter content
5.1.1 Summary of method
Isothiazolinone derivatives react quantitatively with sodium bisulfite, and excess sodium bisulfite reacts with iodine. Excess iodine is titrated with sodium thiosulfate standard titration solution.
The reaction formula is as follows:
CH: + NaHSO.
S--so,Na
NaHSO --12 ---NaHSO +2HI
12+2NazS203-2H1-Na2S,0s
5.1.2 Reagents and materials
5.1.2.1 Standard sodium thiosulfate titration solution: c(Nazs.O.) is about 0.1mol/1. 5.1.2.2 Sodium bisulfite solution (1/2NaHSO) is about 0.5mol/L. Weigh 6.5 sodium bisulfite and dissolve it in 250ml water. This solution is valid for 3d. 5.1.2.3 Iodine solution: c(1/212) is 0.11 mol/L0. 12mol/L (R is H or CI)
Weigh about 15g iodine and about 40 potassium iodide, dissolve in 100mL water, dilute to 1000mL, shake well. Store in a brown bottle. 5.1.2.4 Soluble starch solution: 10g/1. 5.1.3 Analysis steps
Weigh about 1g sample (Class 1) or about 7g sample (Class 2) (accurate to 0.0002g) by reduction method, place in a 250ml iodine volumetric flask pre-added with 30ml water, shake well. Use a pipette to add 10.00ml sulfurous acid Sodium hydrogen solution, let stand for 60 minutes. Use a pipette to add 50.00mL of iodine solution, and immediately titrate with sodium thiosulfate standard titration solution. When the solution turns light yellow, add 1ml-2mL of starch indicator solution, and continue titrating until the blue color disappears, which is the end point. At the same time, perform a blank test.
5.1.4 Expression of analysis results
The active substance content (X) expressed as mass percentage is calculated according to formula (1): 215
HG/T3657—1999
X=Vi-Vo)ex0. 069 6×100
Wherein: V----Volume of sodium thiosulfate standard titration solution consumed by titration test solution, mL.; Volume of sodium thiosulfate standard titration solution consumed by blank test, mL; ....Actual concentration of sodium thiosulfate standard titration solution, mol /Lm-mass of sample, g;
0.0696----Mass of isothiazolinone derivative expressed in grams equivalent to 1.00ml sodium thiosulfate solution [c (Na2SO:) = 1.000mol/1] [calculated as CMI/MI (mass percentage) = 3/1]. 5.1.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results is not more than 0.1% for Class 1 products and not more than 0.02% for Class 2 products.
5.2 Determination of CMI/MI (mass percentage) 5.2.1 Method Summary
Use the difference in the adsorption and desorption rates of CMI and MI on the stationary phase of HPLC to separate them. Calculate their ratio after detection by UV detector.
5.2.2 Reagents and Materials
5.2.2.1 Methanol
5.2.2.2 CMI standard sample, MI standard sample or standard sample containing CMI and MI. 5.2.3 Instruments and Equipment
General laboratory instruments and
High performance liquid chromatograph: equipped with UV detector and data processing system. Operating conditions:
Chromatographic column: YWC-C18 column.
Mobile phase: methanol: water = 40:60 (volume ratio). Flow rate: 1 ml/min.
Detector wavelength: 254nm,
Column temperature: 30C.
5.2.4 Analysis steps
5.2.4.1 Preparation of standard sample solution
Weigh about 0.20g of CMI standard sample and about 0.07g of MI standard sample (or weigh the corresponding amount of standard samples containing CMI and MI) (accurate to 0.0:02g), place in a 50ml volumetric flask, add water to dissolve, dilute to the scale, and shake well. Use a pipette to transfer 1ml~~5mL, place in a 25ml volumetric flask, dilute to the scale with water, shake well for later use. 5.2.4.2 Determination of relative correction factor
Take 20μI standard sample solution for HPLC analysis, and inject the sample at least 5 times continuously. Integrate and calculate the average peak areas SA and SB of the two standards of CMI and MI respectively. The relative correction factor f(A/B) is calculated according to formula (2): f(A/B)=
Seymaa
Where: S, ----- the average value of the chromatographic peak area of the CMI standard obtained by continuously measuring the standard sample solution for more than 5 times, mm2;: the average value of the chromatographic peak area of the MI standard obtained by continuously measuring the standard sample solution for more than 5 times, mm2; S
-the mass of the CMI standard sample, g;
the mass of the MI standard sample, g;
the purity of the CMI standard sample, %;
(2)
-the purity of the MI standard sample, %.
5.2.4.3 Determination
HG/T3657-1999
Weigh about 1.0g of sample (accurate to 0.0002g), place the Class 1 product in a 500mL volumetric flask, and the Class 2 product in a 50ml volumetric flask, dilute with water to the mark, and shake well.
Take 2) μl of the test solution for HPLC analysis, inject the sample at least 3 times continuously, and integrate and calculate the average peak areas S'A and Sn of the CMI and MI components respectively.
5.2.5 Expression of analysis results
CMI/MI (mass percentage) is calculated according to formula (3): CMI/MI=
f(A/B)S'A
Wherein: S\^--the average value of the chromatographic peak area of CMI active matter obtained by continuous determination of the test solution for more than 3 times, mm; S\--the average value of the chromatographic peak area of MI active matter obtained by continuous determination of the test solution for more than 3 times, mm; f(A/B)---the relative correction factor measured in 5.2.4.2. 5.2.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.2. 5.3 Determination of pH value
5.3.1 Instruments and equipment
Acidity meter: accuracy 0.02 pH unit, equipped with saturated calomel reference electrode, glass measuring electrode or composite electrode. 5.3.2 Analysis steps
Pour the sample into a 250mL beaker. Immerse the electrode in the solution and read the pH value on the positioned acidometer. 5.4 Determination of density
5.4.1 Instruments and equipment
5.4.1.1 Density meter: graduation value is 0.001g/cm. 5.4.1.2 Constant temperature water bath: temperature controlled at (20±1)°C. 5.4.1.3 Glass measuring cylinder: 250ml.
5.4.1.4 Thermometer: 0～~50°C, graduation value is 1. 5.4.2 Analysis steps
. (3))
Pour the sample into a clean and dry measuring cylinder without any bubbles, and place the measuring cylinder in a constant temperature water bath at 20°C. After the temperature is constant, slowly place the clean and dry densitometer into the sample. The lower end should be more than 2 cm away from the bottom of the cylinder and should not touch the cylinder wall. The upper end of the densitometer exposed outside the liquid surface should not be stained with liquid for more than 2 to 3 divisions. After the densitometer is stable in the sample, read the scale of the lower edge of the meniscus of the densitometer (except for the densitometer marked with the scale for reading the upper edge of the meniscus), which is the density of the 20C sample. 6 Inspection rules
6.1 The four index items of active matter content, CMI/MI (mass percentage), pH, and density specified in this standard are type inspection items. Under normal production conditions, type inspection shall be carried out at least once every three months. Among them, the three index items of active matter content, pH, and density are factory inspection items, which shall be inspected batch by batch by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard.
6.2 The user unit has the right to inspect and accept the received products in accordance with the provisions of this standard. 6.3 Determine the number of sampling units according to the provisions of 6.6 in GB/T6678--1986. Stir thoroughly when sampling, and use a glass tube or polyethylene plastic tube to insert the sample into 2/3 of the barrel depth. The total amount should not be less than 1000ml. Mix thoroughly, divide into two clean, dry bottles with ground stoppers, and seal. Label the bottles with: manufacturer's name, product name, batch number, sampling date and name of the sampler. One bottle is for inspection, and the other is kept for three months for reference. 6.4 If one indicator in the test results does not meet the requirements of this standard, re-sample from twice the amount of packaging units for verification. If one of the verification results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6.5 Use the rounded value comparison method specified in GB/T1250 to determine whether the test results meet the requirements. 6.6 When the supply and demand parties have any objection to the product quality, they shall handle it in accordance with the provisions of the Quality Law of the People's Republic of China. 7 Marking, packaging, transportation, storage
7.1 The packaging barrels of water treatment agent isothiazolinone derivatives shall be painted with firm markings, including: manufacturer name, product name, trademark, batch number or production date, net content, factory address and the upward mark specified in GB191. 7.2 Each batch of water treatment agent isothiazolinone derivatives shipped shall be accompanied by a quality certificate, including: manufacturer name, product name, trademark, batch number or production date, net content, proof that the product quality complies with this standard and this standard number. 7.3 Water treatment agent isothiazolinone derivatives are packaged in polyethylene plastic barrels with a net content of 25k per barrel, or in iron plastic barrels with a net content of 125kg.200kg per barrel.
7.4 Prevent exposure to sunlight during transportation and store in a ventilated and dry warehouse. 7.5 The storage period of water treatment agent isothiazolinone derivatives is ten months. 8 Safety requirements
Water treatment agent isothiazolinone derivatives are corrosive and can cause burns and allergic dermatitis when in contact with eyes and skin. Protective clothing, glasses and rubber gloves must be worn during operation: Once in contact with the human body, it must be rinsed with plenty of water in a timely manner. 2181 The four indicators specified in this standard, namely, active matter content, CMI/MI (mass percentage), pH, and density, are type inspection items. Under normal production conditions, type inspection shall be carried out at least once every three months. Among them, the three indicators, namely, active matter content, pH, and density, are factory inspection items, which shall be inspected batch by batch by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard.
6.2 The user unit has the right to inspect and accept the received products in accordance with the provisions of this standard. 6.3 Determine the number of sampling units in accordance with the provisions of 6.6 in GB/T6678--1986. Stir thoroughly when sampling, and use a glass tube or polyethylene plastic tube to insert the sample into 2/3 of the barrel depth. The total amount shall not be less than 1000ml. Mix thoroughly, divide into two clean, dry bottles with ground stoppers, and seal. Label the bottles with: manufacturer name, product name, batch number, sampling date, and name of the sampler. One bottle is for inspection, and the other bottle is kept for three months for reference. 6.4 If one of the indicators in the test results does not meet the requirements of this standard, sampling should be repeated from twice the amount of packaging units. If one of the verification results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6.5 The rounded value comparison method specified in GB/T1250 shall be used to determine whether the test results meet the requirements. 6.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Quality Law of the People's Republic of China". 7 Marking, packaging, transportation, storage
7.1 The packaging barrels of water treatment agent isothiazolinone derivatives should be painted with firm markings, including: manufacturer name, product name, trademark, batch number or production date, net content, factory address and the upward mark specified in GB191. 7.2 Each batch of isothiazolinone derivatives of water treatment agents shipped out of the factory should be accompanied by a quality certificate, which includes: manufacturer name, product name, trademark, batch number or production date, net content, proof that the product quality complies with this standard and this standard number. 7.3 Isothiazolinone derivatives of water treatment agents are packaged in polyethylene plastic barrels with a net content of 25k per barrel, or in iron-plastic barrels with a net content of 125kg.200kg per barrel.
7.4 Prevent exposure to sunlight during transportation and store in a ventilated and dry warehouse. 7.5 The storage period of isothiazolinone derivatives of water treatment agents is ten months. 8 Safety requirements
Isothiazolinone derivatives of water treatment agents are corrosive and can cause burns when in contact with eyes and skin, and can also cause allergic dermatitis. Protective clothing, glasses and rubber gloves must be worn during operation: once in contact with the human body, it must be rinsed with plenty of water in time. 2181 The four indicators specified in this standard, namely, active matter content, CMI/MI (mass percentage), pH, and density, are type inspection items. Under normal production conditions, type inspection shall be carried out at least once every three months. Among them, the three indicators, namely, active matter content, pH, and density, are factory inspection items, which shall be inspected batch by batch by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard.
6.2 The user unit has the right to inspect and accept the received products in accordance with the provisions of this standard. 6.3 Determine the number of sampling units in accordance with the provisions of 6.6 in GB/T6678--1986. Stir thoroughly when sampling, and use a glass tube or polyethylene plastic tube to insert the sample into 2/3 of the barrel depth. The total amount shall not be less than 1000ml. Mix thoroughly, divide into two clean, dry bottles with ground stoppers, and seal. Label the bottles with: manufacturer name, product name, batch number, sampling date, and name of the sampler. One bottle is for inspection, and the other bottle is kept for three months for reference. 6.4 If one of the indicators in the test results does not meet the requirements of this standard, sampling should be repeated from twice the amount of packaging units. If one of the verification results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6.5 The rounded value comparison method specified in GB/T1250 shall be used to determine whether the test results meet the requirements. 6.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Quality Law of the People's Republic of China". 7 Marking, packaging, transportation, storage
7.1 The packaging barrels of water treatment agent isothiazolinone derivatives should be painted with firm markings, including: manufacturer name, product name, trademark, batch number or production date, net content, factory address and the upward mark specified in GB191. 7.2 Each batch of isothiazolinone derivatives of water treatment agents shipped out of the factory should be accompanied by a quality certificate, which includes: manufacturer name, product name, trademark, batch number or production date, net content, proof that the product quality complies with this standard and this standard number. 7.3 Isothiazolinone derivatives of water treatment agents are packaged in polyethylene plastic barrels with a net content of 25k per barrel, or in iron-plastic barrels with a net content of 125kg.200kg per barrel.
7.4 Prevent exposure to sunlight during transportation and store in a ventilated and dry warehouse. 7.5 The storage period of isothiazolinone derivatives of water treatment agents is ten months. 8 Safety requirements
Isothiazolinone derivatives of water treatment agents are corrosive and can cause burns when in contact with eyes and skin, and can also cause allergic dermatitis. Protective clothing, glasses and rubber gloves must be worn during operation: once in contact with the human body, it must be rinsed with plenty of water in time. 218
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