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GB 22622-2008: [GB/T 22622-2008] Propamocarb hydrochloride aqueous solution
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[GB/T 22622-2008] Propamocarb hydrochloride aqueous solution
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GB 22622-2008
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Basic data | Standard ID | GB 22622-2008 (GB22622-2008) | | Description (Translated English) | [GB/T 22622-2008] Propamocarb hydrochloride aqueous solution | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.30 | | Word Count Estimation | 12,147 | | Date of Issue | 2008-12-17 | | Date of Implementation | 2009-06-01 | | Quoted Standard | GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 4472; GB/T 19137-2003; GB/T 19136-2003 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 21 of 2008 (No. 134 overall) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard specifies the propamocarb hydrochloride salt agent requirements, test methods and marking, labeling, packaging and storage. This standard applies to Propamocarb (hydrochloride) original drug (or propamocarb hydrochloride parent drug) and the necessary auxiliaries processed into propamocarb hydrochloride salt agent. | GB 22622-2008: [GB/T 22622-2008] Propamocarb hydrochloride aqueous solution---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Propamocarb hydrochloride aqueous solution
ICS 65.100.30
G25
National Standards of People's Republic of China
Propamocarb hydrochloride salt water
Posted 2008-12-17
2009-06-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
The standard Chapter 3, Chapter 5 are mandatory, the rest are recommended.
Appendix A of this standard is an informative annex.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee on Pesticides (SAC/TC133) centralized.
This standard is drafted by. the Ministry of Agriculture.
The main drafters of this standard. Li Youshun, Wu Jinlong, Wang Xiaoli, Chen Tiechun, Wei single force.
Propamocarb hydrochloride salt water
Other active ingredients of the product name, structural formula and basic physicochemical parameters propamocarb hydrochloride as follows.
ISO common name. propamocarbhydrochloride
CAS Registry Number. 25606-41-1
CIPAC digital code. 399
Chemical name. N- [3- (dimethylamino) propyl] carbamic acid ester hydrochloride
Structure.
N (CH2) 3NHCO2 (CH2) 2CH3 · HCl
CH3
CH3
Empirical formula. C9H21ClN2O2
Molecular Weight. 224.7 (according to 2007 international relative atomic mass)
Biological activity. bactericidal
Melting point. 64.2 ℃
Vapour pressure. 3.82 × 10-2 MPa (25 ℃)
Solubility. Water > 500g/L (pH7.0,20 ℃), 656 methanol, dichloromethane > 626, 560 as acetone, ethyl acetate 4.34, toluene
0.14, hexane < 0.01 (both g/L, 20 ℃)
Stability. easy hydrolysis and photolysis, the following 400 ℃ stable
1 Scope
This standard specifies the propamocarb hydrochloride salt water requirements, test methods and marking, labeling, packaging and storage.
This standard applies to the processing by the propamocarb (hydrochloride) original drug (or propamocarb hydrochloride salt of the parent drug) and the necessary aid to the propamocarb hydrochloride
Agent.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
Determination of GB/T 1601 Pesticides pH value
GB/T 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB 3796 pesticide packaging General
GB/T 4472 chemical product density, relative density measurement General
GB/T 19137-2003 Pesticide cryogenic stability Determination
19136-2003 Thermal storage stability of pesticides GB/T Determination
3 Requirements
3.1 Composition and appearance. This product should be compliant propamocarb (hydrochloride) original drug or propamocarb hydrochloride parent drug is made, the appearance of a homogeneous liquid
Body, no obvious suspended solids and sediments.
3.2 propamocarb hydrochloride salt water should meet the requirements of Table 1.
Table 1 propamocarb hydrochloride salt water control project indicators
project
index
722g/L 35.0%
Propamocarb hydrochloride salt mass fraction a /% 66.5 ± 2.5 35.0 ± 1.8
Propamocarb hydrochloride concentration (20 ℃) / (g/L) 722 ± 25 -
Water-insoluble mass fraction /% ≤ 0.3
pH range of 3.0 to 7.0
Dilution stability (diluted 20 times) Qualified
Low temperature stability b a qualified
Thermal storage stability b a qualified
When a dispute arises when quality to propamocarb mass fraction of arbitration.
b low temperature stability, thermal storage stability test under normal production conditions, every 3 months test at least once.
Test Method 4
4.1 Sampling
Carried out according to GB/T 1605-2001 "liquid formulation sampling" method. Determined by sampling a random number table method packages, the final sample size
Not less than 250mL.
4.2 Identification Test
HPLC --- The identification test can be carried out simultaneously with the determination of propamocarb hydrochloride salt mass fraction. In the same chromatographic operation
Under the conditions, the sample solution to a chromatographic retention time and the standard solution of the main peak retention time, the relative difference should
1.5% or less.
4.3 Determination of propamocarb hydrochloride salt mass fraction
4.3.1 Method summary
Sample was dissolved in distilled water to acetonitrile + 1.5% ammonia water as the mobile phase, to use the hybrid silica as filler and alkali resistance condition C18 is not
Stainless steel column and UV detector, other than the standard method of sample propamocarb reverse phase HPLC separation and determination. It can also be used to
Si100 is filling a stainless steel column and UV detector to detect chromatographic operating conditions, see Appendix A.
4.3.2 Reagents and solutions
Acetonitrile. HPLC grade;
Water. The new secondary steam distilled water;
Propamocarb (or propamocarb hydrochloride) standard. a known mass fraction ≥99.0%.
4.3.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector and quantitative injection valve;
Chromatographic data processor or chromatography workstation;
Column. 150mm × 3.9mm (i.d.) Stainless steel column, built XTerraRP18,5μm filler (or other equivalent effect color
The column);
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL;
Ultrasonic cleaner.
4.3.4 HPLC operating conditions
Mobile phase. ψ (acetonitrile .1.5% aqueous ammonia) = 20.80;
The mobile phase flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 210nm;
Injection volume. 20μL;
Retention time. propamocarb about 5.8min.
HPLC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate,
In order to obtain the best results. HPLC view of a typical propamocarb hydrochloride salt water is shown in Figure 1.
1 --- propamocarb.
Figure 1 propamocarb hydrochloride salt water by high performance liquid chromatogram
4.3.5 measuring step
4.3.5.1 Sample solution preparation
Weigh propamocarb (propamocarb hydrochloride) Sample of about 0.05g (accurate to 0.0002g), placed in 100mL volumetric flask with distilled water solution
Solution and diluted to the mark.
4.3.5.2 Sample solution preparation
Weigh containing propamocarb approximately 0.05g sample (accurate to 0.0002g), placed in 100mL volumetric flask, and diluted with distilled water
To the mark. Through 0.45μm membrane filter and set aside.
4.3.5.3 1.5% ammonia preparation
1000mL of distilled water, was added 15mL accurate mass fraction of about 25% aqueous ammonia, shake. Through 0.45μm membrane filter,
stand-by.
4.3.5.4 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles propamocarb relative peak area
After the change of less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.
4.3.6 Calculation
The two doses of the standard solution of two injections of the sample solution and measured before and after the sample solution propamocarb peak areas are averaged. Cream sample
The mass fraction of propamocarb hydrochloride 1 (%) according to equation (1) (standard when propamocarb hydrochloride) or formula (2) (standard of propamocarb time) is calculated,
Mass concentration ρ propamocarb hydrochloride (g/L) according to equation (3) is calculated.
(1)
(2)
Where.
A1 --- the standard solution, the average propamocarb peak area;
A2 --- sample solution, the average propamocarb peak area;
224.7 --- molecular weight propamocarb hydrochloride;
188.3 --- propamocarb molecular weight;
--- Standard samples propamocarb (propamocarb hydrochloride) mass fraction, expressed as a percentage;
4.3.7 allowable difference
The relative deviation of two parallel determination results shall not be greater than ± 2%, whichever is the arithmetic mean as a measurement result.
4.4 Determination of water insoluble mass fraction
4.4.1 Method summary
Samples dissolved in water, all insolubles were filtered off, dried and weighed.
4.4.2 Instruments
Weighing bottle;
Glass sand core crucible. G3;
Suction flask. 100mL;
Oven. 105 ℃ ± 2 ℃.
4.4.3 measuring step
At 105 ℃ in the sand core glass crucible and dried to constant weight (accurate to 0.0002g). Weigh a sample of about 20g (accurate to 0.01g),
Rinsed with 200mL of water was transferred to a graduated cylinder, stoppered, shaken violently, so that soluble dissolved. This solution was sintered glass crucible
Filtered, washed with distilled water residue in the crucible, each with 25mL, washed three times total. Set glass frit crucible and the residue was baked at 105 ℃
Oven dried to constant weight (accurate to 0.0002g).
4.4.4 Calculation
2 water insoluble mass fraction (%), according to equation (4) Calculated.
100 (4)
Where.
According to GB/T 1601 carried out.
4.6 Dilution stability test
4.6.1 Reagents and Instruments
Standard hard water. ρ (Ca
2 ++ Mg2 +) = 342mg/L;
Cylinder. 100mL;
Water bath. 30 ℃ ± 2 ℃;
Pipette. 5mL.
4.6.2 Test procedure
With pipette 5mL sample, placed in 100mL measuring cylinder and diluted to the mark with standard hard water, and mix. Add this cylinder
30 ℃ ± 2 ℃ of water bath, allowed to stand for 1h. As dilution uniform, no precipitation was qualified.
4.7 Low temperature stability test
According to GB/T 19137-2003 "on emulsions and a homogeneous liquid formulation" in volume to precipitate a solid or oil is no more than 0.3mL
qualified.
4.8 Thermal storage stability test
According to GB/T 19136-2003 of "liquid formulation" to. After the thermal storage mass fraction propamocarb hydrochloride should not be lower than the pre-heat storage
95%; the rest of the indicators should remain in line with the requirements of 3.2.
4.9 product testing and acceptance
Shall comply with GB/T 1604's. Limit numerical processing using rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
Label 5.1 propamocarb hydrochloride salt agent shall indicate the mass fraction of propamocarb hydrochloride.
Flag 5.2 propamocarb hydrochloride salt agent, labeling and packaging should comply with the provisions of GB 3796.
5.3 propamocarb hydrochloride salt water available within the plug and cover with a polyester bottle, bottle net content of 200mL, 1000mL etc; outsourcing
Fitted with corrugated boxes or plastic boxes, each containing a net capacity not exceeding 20000mL. Also available upon request or order agreement, the use of other forms of
Packaging, but to comply with the provisions of GB 3796.
5.4 propamocarb hydrochloride salt water package should be stored in ventilated, dry warehouse, stacked manner consistent with safe, convenient handling principles.
5.5 storage, prevent moisture and sunlight, to avoid infiltration of ground; no food, beverages, animal feed-mixing; avoid contact with skin, eye contact
Touch, mouth and nose to prevent inhalation.
5.6 Security. propamocarb hydrochloride salt water is a toxic fungicide harmful. When used, should wear protective gloves, masks, wear dry
Net protective clothing immediately after use with soap and water. The agent contact with skin, wash immediately with soap and water; if splashed into the eyes, should
Rinse immediately with plenty of water; consult a doctor if necessary. If swallowed, do not induce vomiting, consult a doctor, mouth and drink plenty of water, clothes
Activated carbon.
5.7 Warranty. Under the provisions of storage and transportation conditions, warranties of propamocarb hydrochloride salt agent two years from date of manufacture.
Appendix A
(Informative)
Methods (CIPAC method) was measured by liquid chromatography propamocarb hydrochloride salt mass fraction
A. 1 Method summary
+ Water sample was dissolved in methanol, methanol + water + ammonia water as the mobile phase, to use as a filler Si100 stainless steel column and ultraviolet detection
Detector, sample the propamocarb hydrochloride HPLC separation and determination.
A. 2 Reagents and solutions
Methanol. HPLC grade;
Water. The new secondary steam distilled water;
Ammonia solution. 25% (mass fraction);
A mixed solution. [Psi] (methanol. water) = 80.20;
Propamocarb hydrochloride (propamocarb) standard. a known mass fraction ≥99.0%.
A. 3 Instrument
LC. a variable wavelength UV detector and quantitative injection valve;
Chromatographic data processor or chromatography workstation;
Column. LichrosorbSi100,250mm × 4mm (. I.d), 5μm stainless steel column (column or other equivalent effect);
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL.
A. 4 HPLC operating conditions
Mobile phase. [Psi] (methanol. water. aqueous ammonia) = 800.192.8;
The mobile phase flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 210nm;
Injection volume. 10μL;
Retention time. propamocarb about 7.4min.
HPLC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate,
In order to obtain the best results. Typical liquid chromatography is shown in Figure propamocarb hydrochloride salt agent A. 1.
1 --- propamocarb.
Figure A. Figure 1 HPLC propamocarb hydrochloride salt agent
A. 5 measuring step
A. 5.1 preparation of standard solution
Accurately weigh approximately 0.175g (accurate to 0.0002g) of propamocarb hydrochloride standard sample in 100mL volumetric flask, dissolved with a mixed solution
Solution, and set the volume to the mark, shake spare.
A. 5.2 Sample preparation solution
Accurately weighed sample containing about taking propamocarb hydrochloride 0.2g (accurate to 0.0002g), and placed in 100mL flask, with a mixed solution
Dissolve and dilute to the mark, shake spare. Through 0.45μm membrane filter and set aside.
A. 5.3 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles propamocarb relative peak area
After the change of less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.
A. 6 Calculation
The two doses of the standard solution of two injections of the sample solution and measured before and after the sample solution propamocarb peak areas are averaged. Cream sample
The mass fraction of propamocarb hydrochloride 1 (%) according to equation (A.1) (standard when propamocarb hydrochloride) or formula (A.2) (standard of propamocarb time) were
Calculate the mass concentration ρ propamocarb hydrochloride (g/L) according to formula (A.3) calculated as follows.
(A.1)
(A.2)
Where.
A1 --- the standard solution, the average propamocarb peak area;
A2 --- sample solution, the average propamocarb peak area;
224.7 --- molecular weight propamocarb hydrochloride;
188.3 --- propamocarb molecular weight;
--- Standard samples propamocarb (propamocarb hydrochloride) mass fraction, expressed as a percentage;
A. 7 allowable difference
The relative deviation of two parallel determination results shall not be greater than ± 2%, whichever is the arithmetic mean as a measurement result.
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