Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2075-91
J Acid (2-amino-5-naphthol-7-sulfonic acid)
Published on July 17, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1992
Chemical Industry Standard of the People's Republic of China
J Acid (2-amino-5-naphthol-7-sulfonic acid)
Subject Content and Scope of Application
HG2075-91
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation, purchase and storage of J acid. This standard applies to J acid prepared by sulfonation of Tobias acid and oleum, followed by hydrolysis, suction filtration, dissolution, alkali fusion, acidification, and suction filtration. The main use of this product is as an intermediate of azo dyes. Structural formula:
Molecular formula: CioH.NO,S
Relative molecular mass: 239.25 (according to the 1987 international relative atomic mass) 2 Reference standards
Preparation of standard solution for titration analysis (volume analysis) of chemical reagents Preparation of preparations and products used in GB603 chemical reagent test methods 3 Technical requirements
The quality of J acid should meet the requirements of the following table:
Indicator name
J acid content (coupling value)
Acid content (based on 100% J acid)
Di-J acid content (based on 100% J acid)
Note: Di-J acid is a random inspection item, at least once a week. 4 Test method
4.1 Appearance
Measured by visual inspection.
4.2 Determination of J acid content (coupling value)
4.2.1 Principle of the method
Qualified products
Light gray to light brown paste
In a weakly alkaline medium, J acid undergoes quantitative coupling reaction with a diazonium salt standard solution of known concentration. 4.2.2 p-Toluidine diazonium salt method (arbitration method) Approved by the Ministry of Chemical Industry of the People's Republic of China on July 17, 1991 and implemented on January 1, 1992
4.2.2.1 Reagents and solutions
4.2.2.1.1 Hydrochloric acid (GB622): chemically pure. 4.2.2.1.2
Sodium chloride (GB1266): chemically pure.
HG2075—91
4.2.2.1.3 Anhydrous sodium carbonate (GB639) solution: chemically pure, 100g/L. 4.2.2.1.4 Potassium bromide (GB649) solution: chemically pure, 100g/L. Sodium nitrite (GB633) standard solution: chemically pure, c(NaNO2)=0.5mol/L. 4.2.2.1.5
4.2.2.1.6 Standard titration solution of p-toluidine: c(CHgN)=0.5mol/L. Preparation:
Weigh 53.6g p-toluidine (chemically pure) into a beaker, add a small amount of water to mix, add 150mL concentrated hydrochloric acid, stir continuously, add water until completely dissolved, filter, dilute to a 1L brown volumetric flask, mix well, and place in a dark place. Calibration:
Accurately pipette 20.0mL of the above-mentioned p-toluidine solution into a 400mL beaker, add 200mL of water, 10mL of concentrated hydrochloric acid and 10mL of 100g/L potassium bromide, cool to below 15°C, and titrate with sodium nitrite standard titration solution Lc (NaNO2=0.5mol/L) under stirring. During titration, insert the tip of the burette below the liquid surface and titrate at a medium speed. When approaching the end point, lift the burette and add drop by drop until the last drop is still slightly blue on the starch potassium iodide test paper after 5 minutes. Perform a blank test at the same time. Calculation:
=(i-V2)
Wherein: c1——concentration of p-toluidine standard solution, mol/L; c2——concentration of sodium nitrite standard solution, mol/L; V—volume of p-toluidine solution absorbed, mL; V1——volume of sodium nitrite standard solution consumed in titration, mL; V
volume of sodium nitrite standard solution consumed in blank, mL. 4.2.2.1.7 Standard titration solution of p-toluidine diazonium salt: c(C,H,N,CI)=0.1000mol/L. Preparation:
Take a 250mL brown volumetric flask and put the calculated amount of p-toluidine standard titration solution [c(CHgN)=0.5mol/L) (about 50mL) from the burette. Put the calculated amount of sodium nitrite standard titration solution c(NaNO,)=0.5mol/L (about 50mL) into a 100mL conical flask, and add 0.5mL in excess, and cool to 0-5℃. Add the sodium nitrite standard solution to the p-toluidine standard solution while shaking, dilute to the scale with ice water, shake well, and it should show obvious blue on the starch potassium iodide test paper or test solution. Keep at 0-5℃ for 15min before use. The effective time is 6h.
Calculation:
Vs=250X0.100 0
V,=250×0.100.0
Wherein: Vs—the volume of p-toluidine standard solution (4.2.2.1.6) to be added, mL; Cs—the concentration of p-toluidine standard solution, mol/L; V.—the volume of sodium nitrite standard solution (4.2.2.1.5) to be added, mL; c4—the concentration of sodium nitrite standard solution, mol/L. 4.2.2.2 Analysis steps
（2）
（3）
Weigh 1.5~2.5g (accurate to 0.001g) of J acid and add a small amount of water to make a paste. Add 20mL of 100g/L sodium carbonate solution to dissolve it, then add 50mL of 100g/L sodium carbonate solution, add water to a total volume of about 300mL, cool to 0~5℃, and add about 98% of the standard titration solution of p-toluidine diazonium salt [c(CrH>N2CI)=0.1mol/L] at one time with sufficient stirring using a condensing jacket burette. Add 10g of sodium chloride (4.2.2.1.2) to salt out, and continue titrating until the dilute diazonium salt solution (the original solution is diluted 10 times) and the test solution on the filter paper do not produce a light orange-red color at the contact point.
4.2.2.3 Calculation of analysis results
The percentage of J acid (coupling value) r1 is calculated according to formula (4): V.·CX0.2393
Wherein:
1——Percentage of J acid coupling value, %;
Ve—Volume of p-toluidine diazonium salt standard titration solution, mL; C6——Concentration of p-toluidine diazonium salt standard titration solution, mol/L; m——Mass of sample, g;
(4)
0.2393——Mass of J acid in grams equivalent to 1.00mL p-toluidine diazonium salt standard solution c(CHzN,C1)=1.000mol/L).
4.2.2.4 Allowable difference
The difference between two parallel determination results shall not exceed 0.5%. The arithmetic mean shall be taken as the determination result. 4.2.3 Aniline diazonium salt method
4.2.3.1 Reagents and solutions
4.2.3.1.1 Aniline standard titration solution: c(C.HN)=0.5mol/L. Preparation:
Weigh 47g aniline (chemically pure), add 100mL hydrochloric acid, stir well, add water to dissolve, dilute to 1L brown volumetric flask, mix well, and place in a dark place. Accurate calibration Pipette 20.0mL aniline solution into a 250mL beaker, add 100mL water, 10mL 100g/L potassium bromide solution and 5mL hydrochloric acid, cool to below 15℃, and titrate with sodium nitrite standard titration solution [c(NaNO2)=0.5mol/L) under stirring. The titration method and endpoint judgment are the same as 4.2.2.1.6
Calculation method: the same as 4.2.2.1.6.
4.2.3.1.2 Standard titration solution of aniline diazonium salt: c(CcHsN2C1)=0.1000mol/L. Preparation:
Put 50.0mL of aniline standard solution (c(CgHN)=0.5mol/L) in a 250mL beaker, add 10mL of hydrochloric acid and 20mL of 100g/L potassium bromide, titrate at 0～5℃ with sodium nitrite standard titration solution [c(NaNO2)=0.5mol/L] cooled to 05℃, and the end point is when the starch potassium iodide test paper turns blue and the test solution still turns blue on the test paper after 5min. Dilute it in a 250mL brown volumetric flask and shake well. Use at 0～~5℃ within 2h.
Others are the same as 4.2.2.1.
4.2.3.2 Analysis steps
Same as 4.2.2.2.
4.2.3.3 Calculation of analysis results
Same as 4.2.2.3.
4.2.3.4 Allowable difference
Same as 4.2.2.4.
4.3 Determination of acid content
4.3.1 Method summary
Ion pair chromatography. Use a reverse phase chromatographic column and tetramethylammonium bromide as the "counter ion" in the n-propanol-water mobile phase to separate the J acid. The acid content is calculated by the external standard peak height quantitative method. 4.3.2 Instruments
4.3.2.1 Liquid chromatograph:
The infusion pump should meet the following requirements:
Flow range 0.1~5mL/min;
Flow stability ±2%;
Maximum operating pressure 2×10'Pa.
HG2075-91
4.3.2.2 Detector: 254mm single wavelength ultraviolet detector or spectrophotometer with equivalent performance. 4.3.2.3 Injector: Column head or quantitative injection valve. 4.3.2.4 Recorder: 10mV recorder or general chromatography data processor. 4.3.2.5 Ultrasonic generator.
4.3.2.6 Micro syringe: 10mL for column injection. When using a quantitative valve, use a flat-head syringe of corresponding capacity. 4.3.2.7 Glass sand core funnel: No. 5, 250mL. 4.3.3 Reagents and solutions
4.3.3.1 n-propanol,
methanol (GB683);
4.3.3.3 Acid;
4.3.3.4 Ammonia (GB631) solution: chemically pure, (1+4) solution; 4.3.3.5 Hydrochloric acid (GB622) solution: chemically pure, (1+17) solution. 4.3.4 Chromatographic conditions
Mobile phase: n-propanol decahydrate, tetradecamethylammonium bromide-2+98+0.3; Chromatographic column: 5mm×150mm stainless steel tube, wet-filled with 10μm silica gel chemically bonded stationary phase YWG-C1Hs2 (abbreviated as ODS) or other brands of ODS stationary phase with equivalent performance; Detector: wavelength 254nm;
Flow rate: 1.0mL/min;
Sensitivity: 0D, 0.16;
Injection volume: 1uL, diluted accordingly when using a quantitative valve; Recorder paper speed: 300mm/h.
4.3.5 Preparation of standard solution
Weigh 0.0500g of refined acid (100% acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, then dilute with water to a 50mL brown volumetric flask, shake well. Store in a dark place for later use. Pipette 0.10, 0.50, 1.00, 2.00mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.005%, 0.010%, 0.020% (m/m) respectively. This standard solution should be stored in a dark place and has a shelf life of about one month. During use, pay attention to the changes in the correction factor. If there are any changes, re-prepare.
4.3.6 Analysis steps
Weigh 10g of the sample (accurate to 0.01g) into a 100mL beaker, add a small amount of water, mix into a paste, dissolve with 10mL (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water into a 100mL volumetric flask, and shake well. Use a 1mL pipette to draw 1.0mL of the test solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. Its concentration is 1%. Pipette 1uL of the sample solution and the standard solution (4.3.5) with a concentration similar to that of the Y acid in the sample solution or dilute accordingly according to the volume of the quantitative valve and inject. Measure the acid peak heights hs and hi in the spectrum respectively. 4.3.7 Quantitative method
Use the external standard peak height quantitative method.
4.3.8 Calculation of analysis results
HG207591
Figure 1 Legend of amino acid liquid phase chromatogram
1—amino acid; 2—unknown peak; 3 amino acid 4 amino acid Acid content (calculated as 100% amino acid) z: Calculate according to formula (5): 2
Wherein, 2—acid percentage, %;
E. Standard sample solution concentration, %;
h—sample acid peak height, mm;
h.——standard sample acid peak height, mm
m——acid mass, g;
acid content (coupling value), %.
4.3.9 Allowable difference
E,·hX1000
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of di-J acid content
4.4.1 Summary of method
Same as 4.3.1.
4.4.2 Instruments and reagents
Di-J acid: see Appendix A for purification method.
Other conditions are the same as 4.3.2 and 4.3.3.
4.4.3 Chromatographic conditions
Mobile phase: n-propanol decahydrate tetradecamethylammonium bromide = 12+88+0.3. (5)
Other conditions are the same as 4.3.4.
4.4.4 Preparation of standard solution
HG2075-91
Weigh 0.0200g of refined di-J acid (100% di-J acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water to a 100mL brown volumetric flask, shake well, and store in a dark place. Pipette 0.5, 1.0, 1.5, and 2.0mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.002%, 0.003%, and 0.004% (m/m), respectively. The storage method is the same as 4.3.5.
4.4.5 Analysis steps
The same as 4.3.6.
4.4.6 Quantitative method
Same as 4.3.7.
Figure 2 Liquid chromatography of amino acid plus diamino acid
1 Amino amino acid; 2-amino acid; 3-diamino acid
4.4.7 Calculation of analysis results
Same as 4.3.8.
4.4.8 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
5.1 Amino acids shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that all amino acids shipped out of the factory meet the requirements of this standard. Each batch of amino acids shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Diamino acid is a random inspection item, and random inspection shall be carried out at least once a week. 6
HG207591
5.3 The user shall conduct quality inspection on the received J acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each box (barrel) of each batch of products (uniform products), insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts, put them into a sugar porcelain plate, mix the samples carefully, and the total amount of the samples taken shall not be less than 500g, and be divided into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference.
5.5 If one of the inspection results does not meet the requirements of this standard, re-sampling and re-inspection shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of J acid cannot be accepted.
5.6 When the supply and demand parties have disputes over product quality, the two parties shall negotiate to resolve it. Purity determination is based on the p-toluidine diazonium salt method. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging box (barrel) should have firm and clear markings, indicating the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date.
6.2 J acid is packed in wooden boxes or iron barrels lined with plastic bags. The net weight of each box (barrel) is 60 (40) kg, and the bag mouth should be double-tied. 6.3 It should be transported in a clean, roofed vehicle. It must be handled gently when loading and unloading. 6.4 Store in a dry, clean house, prevent exposure to the sun and rain, and place the box (barrel) with the mouth facing upward to prevent product leakage. 7
HG2075—91
Appendix A
Bis-J acid purification method
(Supplement)
Dissolve industrial bis-J acid in boiling water until saturated, filter while hot, cool the filtrate naturally, filter after bis-J acid crystals are precipitated, and take the filter cake. Repeat the above steps until there is no impurity under liquid chromatography conditions. Dry the filter cake at 7080℃, place it in a brown ground-mouth bottle, seal it for storage, and determine its content at the same time.
Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Li Qinnan.1 Method Summary
Ion pair chromatography. Use reverse phase chromatographic column, n-propanol-water mobile phase with tetramethylammonium bromide as "counter ion" to separate J acid. The acid content is calculated by external standard peak height quantitative method. 4.3.2 Instruments
4.3.2.1 Liquid chromatograph:
The infusion pump should meet the following requirements:
Flow range 0.1~5mL/min;
Flow stability ±2%;
Maximum operating pressure 2×10'Pa.
HG2075-91
4.3.2.2 Detector: 254mm single wavelength ultraviolet detector or spectrophotometer with equivalent performance. 4.3.2.3 Injector: column head or quantitative injection valve. 4.3.2.4 Recorder: 10mV recorder or general chromatography data processor. 4.3.2.5 Ultrasonicator.
4.3.2.6 Microsyringe: 10mL for column injection. When using a quantitative valve, use a flat-head syringe of corresponding capacity. 4.3.2.7 Glass sand core funnel: No. 5, 250mL. 4.3.3 Reagents and solutions
4.3.3.1 n-propanol,
methanol (GB683);
4.3.3.3 Acid;
4.3.3.4 Ammonia (GB631) solution: chemically pure, (1+4) solution; 4.3.3.5 Hydrochloric acid (GB622) solution: chemically pure, (1+17) solution. 4.3.4 Chromatographic conditions
Mobile phase: n-propanol decahydrate, tetradecamethylammonium bromide-2+98+0.3; Chromatographic column: 5mm×150mm stainless steel tube, wet-filled with 10μm silica gel chemically bonded stationary phase YWG-C1Hs2 (abbreviated as ODS) or other brands of ODS stationary phase with equivalent performance; Detector: wavelength 254nm;
Flow rate: 1.0mL/min;
Sensitivity: 0D, 0.16;
Injection volume: 1uL, diluted accordingly when using a quantitative valve; Recorder paper speed: 300mm/h.
4.3.5 Preparation of standard solution
Weigh 0.0500g of refined acid (100% acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, then dilute with water to a 50mL brown volumetric flask, shake well. Store in a dark place for later use. Pipette 0.10, 0.50, 1.00, 2.00mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.005%, 0.010%, 0.020% (m/m) respectively. This standard solution should be stored in a dark place and has a shelf life of about one month. During use, pay attention to the changes in the correction factor. If there are any changes, re-prepare.
4.3.6 Analysis steps
Weigh 10g of the sample (accurate to 0.01g) into a 100mL beaker, add a small amount of water, mix into a paste, dissolve with 10mL (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water into a 100mL volumetric flask, and shake well. Use a 1mL pipette to draw 1.0mL of the test solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. Its concentration is 1%. Pipette 1uL of the sample solution and the standard solution (4.3.5) with a concentration similar to that of the Y acid in the sample solution or dilute accordingly according to the volume of the quantitative valve and inject. Measure the acid peak heights hs and hi in the spectrum respectively. 4.3.7 Quantitative method
Use the external standard peak height quantitative method.
4.3.8 Calculation of analysis results
HG207591
Figure 1 Legend of amino acid liquid phase chromatogram
1—amino acid; 2—unknown peak; 3 amino acid 4 amino acid Acid content (calculated as 100% amino acid) z: Calculate according to formula (5): 2
Wherein, 2—acid percentage, %;
E. Standard sample solution concentration, %;
h—sample acid peak height, mm;
h.——standard sample acid peak height, mm
m——acid mass, g;
acid content (coupling value), %.
4.3.9 Allowable difference
E,·hX1000
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of di-J acid contentwww.bzxz.net
4.4.1 Summary of method
Same as 4.3.1.
4.4.2 Instruments and reagents
Di-J acid: see Appendix A for purification method.
Other conditions are the same as 4.3.2 and 4.3.3.
4.4.3 Chromatographic conditions
Mobile phase: n-propanol decahydrate tetradecamethylammonium bromide = 12+88+0.3. (5)
Other conditions are the same as 4.3.4.
4.4.4 Preparation of standard solution
HG2075-91
Weigh 0.0200g of refined di-J acid (100% di-J acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water to a 100mL brown volumetric flask, shake well, and store in a dark place. Pipette 0.5, 1.0, 1.5, and 2.0mL of the above solution into 10mL brown volumetric flasks, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.002%, 0.003%, and 0.004% (m/m), respectively. The storage method is the same as 4.3.5.
4.4.5 Analysis steps
The same as 4.3.6.
4.4.6 Quantitative method
Same as 4.3.7.
Figure 2 Liquid chromatography of amino acid plus diamino acid
1 Amino amino acid; 2-amino acid; 3-diamino acid
4.4.7 Calculation of analysis results
Same as 4.3.8.
4.4.8 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
5.1 Amino acids shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that all amino acids shipped out of the factory meet the requirements of this standard. Each batch of amino acids shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Diamino acid is a random inspection item, and random inspection shall be carried out at least once a week. 6
HG207591
5.3 The user shall conduct quality inspection on the received J acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each box (barrel) of each batch of products (uniform products), insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts, put them into a sugar porcelain plate, mix the samples carefully, and the total amount of the samples taken shall not be less than 500g, and be divided into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference.
5.5 If one of the inspection results does not meet the requirements of this standard, re-sampling and re-inspection shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of J acid cannot be accepted.
5.6 When the supply and demand parties have disputes over product quality, the two parties shall negotiate to resolve it. Purity determination is based on the p-toluidine diazonium salt method. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging box (barrel) should have firm and clear markings, indicating the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date.
6.2 J acid is packed in wooden boxes or iron barrels lined with plastic bags. The net weight of each box (barrel) is 60 (40) kg, and the bag mouth should be double-tied. 6.3 It should be transported in a clean, roofed vehicle. It must be handled gently when loading and unloading. 6.4 Store in a dry, clean house, prevent exposure to the sun and rain, and place the box (barrel) with the mouth facing upward to prevent product leakage. 7
HG2075—91
Appendix A
Bis-J acid purification method
(Supplement)
Dissolve industrial bis-J acid in boiling water until saturated, filter while hot, cool the filtrate naturally, filter after bis-J acid crystals are precipitated, and take the filter cake. Repeat the above steps until there is no impurity under liquid chromatography conditions. Dry the filter cake at 7080℃, place it in a brown ground-mouth bottle, seal it for storage, and determine its content at the same time.
Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Li Qinnan.1 Method Summary
Ion pair chromatography. Use reverse phase chromatographic column, n-propanol-water mobile phase with tetramethylammonium bromide as "counter ion" to separate J acid. The acid content is calculated by external standard peak height quantitative method. 4.3.2 Instruments
4.3.2.1 Liquid chromatograph:
The infusion pump should meet the following requirements:
Flow range 0.1~5mL/min;
Flow stability ±2%;
Maximum operating pressure 2×10'Pa.
HG2075-91
4.3.2.2 Detector: 254mm single wavelength ultraviolet detector or spectrophotometer with equivalent performance. 4.3.2.3 Injector: column head or quantitative injection valve. 4.3.2.4 Recorder: 10mV recorder or general chromatography data processor. 4.3.2.5 Ultrasonicator.
4.3.2.6 Microsyringe: 10mL for column injection. When using a quantitative valve, use a flat-head syringe of corresponding capacity. 4.3.2.7 Glass sand core funnel: No. 5, 250mL. 4.3.3 Reagents and solutions
4.3.3.1 n-propanol,
methanol (GB683);
4.3.3.3 Acid;
4.3.3.4 Ammonia (GB631) solution: chemically pure, (1+4) solution; 4.3.3.5 Hydrochloric acid (GB622) solution: chemically pure, (1+17) solution. 4.3.4 Chromatographic conditions
Mobile phase: n-propanol decahydrate, tetradecamethylammonium bromide-2+98+0.3; Chromatographic column: 5mm×150mm stainless steel tube, wet-filled with 10μm silica gel chemically bonded stationary phase YWG-C1Hs2 (abbreviated as ODS) or other brands of ODS stationary phase with equivalent performance; Detector: wavelength 254nm;
Flow rate: 1.0mL/min;
Sensitivity: 0D, 0.16;
Injection volume: 1uL, diluted accordingly when using a quantitative valve; Recorder paper speed: 300mm/h.
4.3.5 Preparation of standard solution
Weigh 0.0500g of refined acid (100% acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, then dilute with water to a 50mL brown volumetric flask, shake well. Store in a dark place for later use. Pipette 0.10, 0.50, 1.00, 2.00mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.005%, 0.010%, 0.020% (m/m) respectively. This standard solution should be stored in a dark place and has a shelf life of about one month. During use, pay attention to the changes in the correction factor. If there are any changes, re-prepare.
4.3.6 Analysis steps
Weigh 10g of the sample (accurate to 0.01g) into a 100mL beaker, add a small amount of water, mix into a paste, dissolve with 10mL (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water into a 100mL volumetric flask, and shake well. Use a 1mL pipette to draw 1.0mL of the test solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. Its concentration is 1%. Pipette 1uL of the sample solution and the standard solution (4.3.5) with a concentration similar to that of the Y acid in the sample solution or dilute accordingly according to the volume of the quantitative valve and inject. Measure the acid peak heights hs and hi in the spectrum respectively. 4.3.7 Quantitative method
Use the external standard peak height quantitative method.
4.3.8 Calculation of analysis results
HG207591
Figure 1 Legend of amino acid liquid phase chromatogram
1—amino acid; 2—unknown peak; 3 amino acid 4 amino acid Acid content (calculated as 100% amino acid) z: Calculate according to formula (5): 2
Wherein, 2—acid percentage, %;
E. Standard sample solution concentration, %;
h—sample acid peak height, mm;
h.——standard sample acid peak height, mm
m——acid mass, g;
acid content (coupling value), %.
4.3.9 Allowable difference
E,·hX1000
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of di-J acid content
4.4.1 Summary of method
Same as 4.3.1.
4.4.2 Instruments and reagents
Di-J acid: see Appendix A for purification method.
Other conditions are the same as 4.3.2 and 4.3.3.
4.4.3 Chromatographic conditions
Mobile phase: n-propanol decahydrate tetradecamethylammonium bromide = 12+88+0.3. (5)
Other conditions are the same as 4.3.4.
4.4.4 Preparation of standard solution
HG2075-91
Weigh 0.0200g of refined di-J acid (100% di-J acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water to a 100mL brown volumetric flask, shake well, and store in a dark place. Pipette 0.5, 1.0, 1.5, and 2.0mL of the above solution into 10mL brown volumetric flasks, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.002%, 0.003%, and 0.004% (m/m), respectively. The storage method is the same as 4.3.5.
4.4.5 Analysis steps
The same as 4.3.6.
4.4.6 Quantitative method
Same as 4.3.7.
Figure 2 Liquid chromatography of amino acid plus diamino acid
1 Amino amino acid; 2-amino acid; 3-diamino acid
4.4.7 Calculation of analysis results
Same as 4.3.8.
4.4.8 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
5.1 Amino acids shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that all amino acids shipped out of the factory meet the requirements of this standard. Each batch of amino acids shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Diamino acid is a random inspection item, and random inspection shall be carried out at least once a week. 6
HG207591
5.3 The user shall conduct quality inspection on the received J acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each box (barrel) of each batch of products (uniform products), insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts, put them into a sugar porcelain plate, mix the samples carefully, and the total amount of the samples taken shall not be less than 500g, and be divided into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference.
5.5 If one of the inspection results does not meet the requirements of this standard, re-sampling and re-inspection shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of J acid cannot be accepted.
5.6 When the supply and demand parties have disputes over product quality, the two parties shall negotiate to resolve it. Purity determination is based on the p-toluidine diazonium salt method. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging box (barrel) should have firm and clear markings, indicating the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date.
6.2 J acid is packed in wooden boxes or iron barrels lined with plastic bags. The net weight of each box (barrel) is 60 (40) kg, and the bag mouth should be double-tied. 6.3 It should be transported in a clean, roofed vehicle. It must be handled gently when loading and unloading. 6.4 Store in a dry, clean house, prevent exposure to the sun and rain, and place the box (barrel) with the mouth facing upward to prevent product leakage. 7
HG2075—91
Appendix A
Bis-J acid purification method
(Supplement)
Dissolve industrial bis-J acid in boiling water until saturated, filter while hot, cool the filtrate naturally, filter after bis-J acid crystals are precipitated, and take the filter cake. Repeat the above steps until there is no impurity under liquid chromatography conditions. Dry the filter cake at 7080℃, place it in a brown ground-mouth bottle, seal it for storage, and determine its content at the same time.
Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Li Qinnan.1~5mL/min;
Flow stability ±2%;
Maximum operating pressure 2×10'Pa.
HG2075-91
4.3.2.2 Detector: 254mm single wavelength UV detector or spectrophotometer with equivalent performance. 4.3.2.3 Injector: Column head or quantitative injection valve. 4.3.2.4 Recorder: 10mV recorder or general chromatography data processor. 4.3.2.5 Ultrasonic generator.
4.3.2.6 Micro syringe: 10mL for column head injection. When using quantitative valve, use a flat-head syringe of corresponding capacity. 4.3.2.7 Glass sand core funnel: No. 5, 250mL. 4.3.3 Reagents and solutions
4.3.3.1 n-Propanol,
Methanol (GB683);
4.3.3.3 Acid;
4.3.3.4 Ammonia water (GB631) solution: chemically pure, (1+4) solution; 4.3.3.5 Hydrochloric acid (GB622) solution: chemically pure, (1+17) solution. 4.3.4 Chromatographic conditions
Mobile phase: n-propanol decahydrate, tetradecamethylammonium bromide-2+98+0.3; Chromatographic column: 5mm×150mm stainless steel tube, wet-filled with 10μm silica gel chemically bonded stationary phase YWG-C1Hs2 (abbreviated as ODS) or other brands of ODS stationary phase with equivalent performance; Detector: wavelength 254nm;
Flow rate: 1.0mL/min;
Sensitivity: 0D, 0.16;
Injection volume: 1uL, diluted accordingly when using a quantitative valve; Recorder paper speed: 300mm/h.
4.3.5 Preparation of standard solution
Weigh 0.0500g of refined acid (100% acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, then dilute with water to a 50mL brown volumetric flask, shake well. Store in a dark place for later use. Pipette 0.10, 0.50, 1.00, 2.00mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.005%, 0.010%, 0.020% (m/m) respectively. This standard solution should be stored in a dark place and has a shelf life of about one month. During use, pay attention to the changes in the correction factor. If there are any changes, re-prepare.
4.3.6 Analysis steps
Weigh 10g of the sample (accurate to 0.01g) into a 100mL beaker, add a small amount of water, mix into a paste, dissolve with 10mL (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water into a 100mL volumetric flask, and shake well. Use a 1mL pipette to draw 1.0mL of the test solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. Its concentration is 1%. Pipette 1uL of the sample solution and the standard solution (4.3.5) with a concentration similar to that of the Y acid in the sample solution or dilute accordingly according to the volume of the quantitative valve and inject. Measure the acid peak heights hs and hi in the spectrum respectively. 4.3.7 Quantitative method
Use the external standard peak height quantitative method.
4.3.8 Calculation of analysis results
HG207591
Figure 1 Legend of amino acid liquid phase chromatogram
1—amino acid; 2—unknown peak; 3 amino acid 4 amino acid Acid content (calculated as 100% amino acid) z: Calculate according to formula (5): 2
Wherein, 2—acid percentage, %;
E. Standard sample solution concentration, %;
h—sample acid peak height, mm;
h.——standard sample acid peak height, mm
m——acid mass, g;
acid content (coupling value), %.
4.3.9 Allowable difference
E,·hX1000
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of di-J acid content
4.4.1 Summary of method
Same as 4.3.1.
4.4.2 Instruments and reagents
Di-J acid: see Appendix A for purification method.
Other conditions are the same as 4.3.2 and 4.3.3.
4.4.3 Chromatographic conditions
Mobile phase: n-propanol decahydrate tetradecamethylammonium bromide = 12+88+0.3. (5)
Other conditions are the same as 4.3.4.
4.4.4 Preparation of standard solution
HG2075-91
Weigh 0.0200g of refined di-J acid (100% di-J acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water to a 100mL brown volumetric flask, shake well, and store in a dark place. Pipette 0.5, 1.0, 1.5, and 2.0mL of the above solution into 10mL brown volumetric flasks, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.002%, 0.003%, and 0.004% (m/m), respectively. The storage method is the same as 4.3.5.
4.4.5 Analysis steps
The same as 4.3.6.
4.4.6 Quantitative method
Same as 4.3.7.
Figure 2 Liquid chromatography of amino acid plus diamino acid
1 Amino amino acid; 2-amino acid; 3-diamino acid
4.4.7 Calculation of analysis results
Same as 4.3.8.
4.4.8 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
5.1 Amino acids shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that all amino acids shipped out of the factory meet the requirements of this standard. Each batch of amino acids shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Diamino acid is a random inspection item, and random inspection shall be carried out at least once a week. 6
HG207591
5.3 The user shall conduct quality inspection on the received J acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each box (barrel) of each batch of products (uniform products), insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts, put them into a sugar porcelain plate, mix the samples carefully, and the total amount of the samples taken shall not be less than 500g, and be divided into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference.
5.5 If one of the inspection results does not meet the requirements of this standard, re-sampling and re-inspection shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of J acid cannot be accepted.
5.6 When the supply and demand parties have disputes over product quality, the two parties shall negotiate to resolve it. Purity determination is based on the p-toluidine diazonium salt method. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging box (barrel) should have firm and clear markings, indicating the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date.
6.2 J acid is packed in wooden boxes or iron barrels lined with plastic bags. The net weight of each box (barrel) is 60 (40) kg, and the bag mouth should be double-tied. 6.3 It should be transported in a clean, roofed vehicle. It must be handled gently when loading and unloading. 6.4 Store in a dry, clean house, prevent exposure to the sun and rain, and place the box (barrel) with the mouth facing upward to prevent product leakage. 7
HG2075—91
Appendix A
Bis-J acid purification method
(Supplement)
Dissolve industrial bis-J acid in boiling water until saturated, filter while hot, cool the filtrate naturally, filter after bis-J acid crystals are precipitated, and take the filter cake. Repeat the above steps until there is no impurity under liquid chromatography conditions. Dry the filter cake at 7080℃, place it in a brown ground-mouth bottle, seal it for storage, and determine its content at the same time.
Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Li Qinnan.1~5mL/min;
Flow stability ±2%;
Maximum operating pressure 2×10'Pa.
HG2075-91
4.3.2.2 Detector: 254mm single wavelength UV detector or spectrophotometer with equivalent performance. 4.3.2.3 Injector: Column head or quantitative injection valve. 4.3.2.4 Recorder: 10mV recorder or general chromatography data processor. 4.3.2.5 Ultrasonic generator.
4.3.2.6 Micro syringe: 10mL for column head injection. When using quantitative valve, use a flat-head syringe of corresponding capacity. 4.3.2.7 Glass sand core funnel: No. 5, 250mL. 4.3.3 Reagents and solutions
4.3.3.1 n-Propanol,
Methanol (GB683);
4.3.3.3 Acid;
4.3.3.4 Ammonia water (GB631) solution: chemically pure, (1+4) solution; 4.3.3.5 Hydrochloric acid (GB622) solution: chemically pure, (1+17) solution. 4.3.4 Chromatographic conditions
Mobile phase: n-propanol decahydrate, tetradecamethylammonium bromide-2+98+0.3; Chromatographic column: 5mm×150mm stainless steel tube, wet-filled with 10μm silica gel chemically bonded stationary phase YWG-C1Hs2 (abbreviated as ODS) or other brands of ODS stationary phase with equivalent performance; Detector: wavelength 254nm;
Flow rate: 1.0mL/min;
Sensitivity: 0D, 0.16;
Injection volume: 1uL, diluted accordingly when using a quantitative valve; Recorder paper speed: 300mm/h.
4.3.5 Preparation of standard solution
Weigh 0.0500g of refined acid (100% acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, then dilute with water to a 50mL brown volumetric flask, shake well. Store in a dark place for later use. Pipette 0.10, 0.50, 1.00, 2.00mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.005%, 0.010%, 0.020% (m/m) respectively. This standard solution should be stored in a dark place and has a shelf life of about one month. During use, pay attention to the changes in the correction factor. If there are any changes, re-prepare.
4.3.6 Analysis steps
Weigh 10g of the sample (accurate to 0.01g) into a 100mL beaker, add a small amount of water, mix into a paste, dissolve with 10mL (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water into a 100mL volumetric flask, and shake well. Use a 1mL pipette to draw 1.0mL of the test solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. Its concentration is 1%. Pipette 1uL of the sample solution and the standard solution (4.3.5) with a concentration similar to that of the Y acid in the sample solution or dilute accordingly according to the volume of the quantitative valve and inject. Measure the acid peak heights hs and hi in the spectrum respectively. 4.3.7 Quantitative method
Use the external standard peak height quantitative method.
4.3.8 Calculation of analysis results
HG207591
Figure 1 Legend of amino acid liquid phase chromatogram
1—amino acid; 2—unknown peak; 3 amino acid 4 amino acid Acid content (calculated as 100% amino acid) z: Calculate according to formula (5): 2
Wherein, 2—acid percentage, %;
E. Standard sample solution concentration, %;
h—sample acid peak height, mm;
h.——standard sample acid peak height, mm
m——acid mass, g;
acid content (coupling value), %.
4.3.9 Allowable difference
E,·hX1000
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of di-J acid content
4.4.1 Summary of method
Same as 4.3.1.
4.4.2 Instruments and reagents
Di-J acid: see Appendix A for purification method.
Other conditions are the same as 4.3.2 and 4.3.3.
4.4.3 Chromatographic conditions
Mobile phase: n-propanol decahydrate tetradecamethylammonium bromide = 12+88+0.3. (5)
Other conditions are the same as 4.3.4.
4.4.4 Preparation of standard solution
HG2075-91
Weigh 0.0200g of refined di-J acid (100% di-J acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water to a 100mL brown volumetric flask, shake well, and store in a dark place. Pipette 0.5, 1.0, 1.5, and 2.0mL of the above solution into 10mL brown volumetric flasks, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.002%, 0.003%, and 0.004% (m/m), respectively. The storage method is the same as 4.3.5.
4.4.5 Analysis steps
The same as 4.3.6.
4.4.6 Quantitative method
Same as 4.3.7.
Figure 2 Liquid chromatography of amino acid plus diamino acid
1 Amino amino acid; 2-amino acid; 3-diamino acid
4.4.7 Calculation of analysis results
Same as 4.3.8.
4.4.8 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
5.1 Amino acids shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that all amino acids shipped out of the factory meet the requirements of this standard. Each batch of amino acids shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Diamino acid is a random inspection item, and random inspection shall be carried out at least once a week. 6
HG207591
5.3 The user shall conduct quality inspection on the received J acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each box (barrel) of each batch of products (uniform products), insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts, put them into a sugar porcelain plate, mix the samples carefully, and the total amount of the samples taken shall not be less than 500g, and be divided into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference.
5.5 If one of the inspection results does not meet the requirements of this standard, re-sampling and re-inspection shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of J acid cannot be accepted.
5.6 When the supply and demand parties have disputes over product quality, the two parties shall negotiate to resolve it. Purity determination is based on the p-toluidine diazonium salt method. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging box (barrel) should have firm and clear markings, indicating the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date.
6.2 J acid is packed in wooden boxes or iron barrels lined with plastic bags. The net weight of each box (barrel) is 60 (40) kg, and the bag mouth should be double-tied. 6.3 It should be transported in a clean, roofed vehicle. It must be handled gently when loading and unloading. 6.4 Store in a dry, clean house, prevent exposure to the sun and rain, and place the box (barrel) with the mouth facing upward to prevent product leakage. 7
HG2075—91
Appendix A
Bis-J acid purification method
(Supplement)
Dissolve industrial bis-J acid in boiling water until saturated, filter while hot, cool the filtrate naturally, filter after bis-J acid crystals are precipitated, and take the filter cake. Repeat the above steps until there is no impurity under liquid chromatography conditions. Dry the filter cake at 7080℃, place it in a brown ground-mouth bottle, seal it for storage, and determine its content at the same time.
Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Li Qinnan.7 Glass frit funnel: No. 5, 250 mL. 4.3.3 Reagents and solutions
4.3.3.1 n-propanol,
methanol (GB683);
4.3.3.3 Acid;
4.3.3.4 Ammonia solution (GB631): chemically pure, (1+4) solution; 4.3.3.5 Hydrochloric acid (GB622): chemically pure, (1+17) solution. 4.3.4 Chromatographic conditions
Mobile phase: n-propanol decahydrate, tetradecamethylammonium bromide-2+98+0.3; Chromatographic column: 5mm×150mm stainless steel tube, wet-filled with 10μm silica gel chemically bonded stationary phase YWG-C1Hs2 (abbreviated as ODS) or other brands of ODS stationary phase with equivalent performance; Detector: wavelength 254nm;
Flow rate: 1.0mL/min;
Sensitivity: 0D, 0.16;
Injection volume: 1uL, diluted accordingly when using a quantitative valve; Recorder paper speed: 300mm/h.
4.3.5 Preparation of standard solution
Weigh 0.0500g of refined acid (100% acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, then dilute with water to a 50mL brown volumetric flask, shake well. Store in a dark place for later use. Pipette 0.10, 0.50, 1.00, 2.00mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.005%, 0.010%, 0.020% (m/m) respectively. This standard solution should be stored in a dark place and has a shelf life of about one month. During use, pay attention to the changes in the correction factor. If there are any changes, re-prepare.
4.3.6 Analysis steps
Weigh 10g of the sample (accurate to 0.01g) into a 100mL beaker, add a small amount of water, mix into a paste, dissolve with 10mL (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water into a 100mL volumetric flask, and shake well. Use a 1mL pipette to draw 1.0mL of the test solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. Its concentration is 1%. Pipette 1uL of the sample solution and the standard solution (4.3.5) with a concentration similar to that of the Y acid in the sample solution or dilute accordingly according to the volume of the quantitative valve and inject. Measure the acid peak heights hs and hi in the spectrum respectively. 4.3.7 Quantitative method
Use the external standard peak height quantitative method.
4.3.8 Calculation of analysis results
HG207591
Figure 1 Legend of amino acid liquid phase chromatogram
1—amino acid; 2—unknown peak; 3 amino acid 4 amino acid Acid content (calculated as 100% amino acid) z: Calculate according to formula (5): 2
Wherein, 2—acid percentage, %;
E. Standard sample solution concentration, %;
h—sample acid peak height, mm;
h.——standard sample acid peak height, mm
m——acid mass, g;
acid content (coupling value), %.
4.3.9 Allowable difference
E,·hX1000
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of di-J acid content
4.4.1 Summary of method
Same as 4.3.1.
4.4.2 Instruments and reagents
Di-J acid: see Appendix A for purification method.
Other conditions are the same as 4.3.2 and 4.3.3.
4.4.3 Chromatographic conditions
Mobile phase: n-propanol decahydrate tetradecamethylammonium bromide = 12+88+0.3. (5)
Other conditions are the same as 4.3.4.
4.4.4 Preparation of standard solution
HG2075-91
Weigh 0.0200g of refined di-J acid (100% di-J acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water to a 100mL brown volumetric flask, shake well, and store in a dark place. Pipette 0.5, 1.0, 1.5, and 2.0mL of the above solution into 10mL brown volumetric flasks, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.002%, 0.003%, and 0.004% (m/m), respectively. The storage method is the same as 4.3.5.
4.4.5 Analysis steps
The same as 4.3.6.
4.4.6 Quantitative method
Same as 4.3.7.
Figure 2 Liquid chromatography of amino acid plus diamino acid
1 Amino amino acid; 2-amino acid; 3-diamino acid
4.4.7 Calculation of analysis results
Same as 4.3.8.
4.4.8 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
5.1 Amino acids shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that all amino acids shipped out of the factory meet the requirements of this standard. Each batch of amino acids shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Diamino acid is a random inspection item, and random inspection shall be carried out at least once a week. 6
HG207591
5.3 The user shall conduct quality inspection on the received J acid in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.4 Sampling method: From each box (barrel) of each batch of products (uniform products), insert a stainless steel sampler vertically to the bottom, take out the samples including the upper, middle and lower parts, put them into a sugar porcelain plate, mix the samples carefully, and the total amount of the samples taken shall not be less than 500g, and be divided into two clean, dry, wide-mouth bottles with ground stoppers. Labels are attached to the bottles, indicating the name of the manufacturer, product name, batch number and sampling date. One bottle is used for inspection and one bottle is kept for reference.
5.5 If one of the inspection results does not meet the requirements of this standard, re-sampling and re-inspection shall be carried out. If the results still do not meet the requirements of this standard, the whole batch of J acid cannot be accepted.
5.6 When the supply and demand parties have disputes over product quality, the two parties shall negotiate to resolve it. Purity determination is based on the p-toluidine diazonium salt method. 6 Marking, packaging, transportation, purchase and storage
6.1 The packaging box (barrel) should have firm and clear markings, indicating the manufacturer's name, product name, trademark, batch number, gross weight, net weight, grade and production date.
6.2 J acid is packed in wooden boxes or iron barrels lined with plastic bags. The net weight of each box (barrel) is 60 (40) kg, and the bag mouth should be double-tied. 6.3 It should be transported in a clean, roofed vehicle. It must be handled gently when loading and unloading. 6.4 Store in a dry, clean house, prevent exposure to the sun and rain, and place the box (barrel) with the mouth facing upward to prevent product leakage. 7
HG2075—91
Appendix A
Bis-J acid purification method
(Supplement)
Dissolve industrial bis-J acid in boiling water until saturated, filter while hot, cool the filtrate naturally, filter after bis-J acid crystals are precipitated, and take the filter cake. Repeat the above steps until there is no impurity under liquid chromatography conditions. Dry the filter cake at 7080℃, place it in a brown ground-mouth bottle, seal it for storage, and determine its content at the same time.
Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Nanjing Chemical Plant of the Ministry of Chemical Industry. The main drafter of this standard is Li Qinnan.7 Glass frit funnel: No. 5, 250 mL. 4.3.3 Reagents and solutions
4.3.3.1 n-propanol,
methanol (GB683);
4.3.3.3 Acid;
4.3.3.4 Ammonia solution (GB631): chemically pure, (1+4) solution; 4.3.3.5 Hydrochloric acid (GB622): chemically pure, (1+17) solution. 4.3.4 Chromatographic conditions
Mobile phase: n-propanol decahydrate, tetradecamethylammonium bromide-2+98+0.3; Chromatographic column: 5mm×150mm stainless steel tube, wet-filled with 10μm silica gel chemically bonded stationary phase YWG-C1Hs2 (abbreviated as ODS) or other brands of ODS stationary phase with equivalent performance; Detector: wavelength 254nm;
Flow rate: 1.0mL/min;
Sensitivity: 0D, 0.16;
Injection volume: 1uL, diluted accordingly when using a quantitative valve; Recorder paper speed: 300mm/h.
4.3.5 Preparation of standard solution
Weigh 0.0500g of refined acid (100% acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, then dilute with water to a 50mL brown volumetric flask, shake well. Store in a dark place for later use. Pipette 0.10, 0.50, 1.00, 2.00mL of the above solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.005%, 0.010%, 0.020% (m/m) respectively. This standard solution should be stored in a dark place and has a shelf life of about one month. During use, pay attention to the changes in the correction factor. If there are any changes, re-prepare.
4.3.6 Analysis steps
Weigh 10g of the sample (accurate to 0.01g) into a 100mL beaker, add a small amount of water, mix into a paste, dissolve with 10mL (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water into a 100mL volumetric flask, and shake well. Use a 1mL pipette to draw 1.0mL of the test solution into a 10mL brown volumetric flask, dilute to the scale with mobile phase, and shake well. Its concentration is 1%. Pipette 1uL of the sample solution and the standard solution (4.3.5) with a concentration similar to that of the Y acid in the sample solution or dilute accordingly according to the volume of the quantitative valve and inject. Measure the acid peak heights hs and hi in the spectrum respectively. 4.3.7 Quantitative method
Use the external standard peak height quantitative method.
4.3.8 Calculation of analysis results
HG207591
Figure 1 Legend of amino acid liquid phase chromatogram
1—amino acid; 2—unknown peak; 3 amino acid 4 amino acid Acid content (calculated as 100% amino acid) z: Calculate according to formula (5): 2
Wherein, 2—acid percentage, %;
E. Standard sample solution concentration, %;
h—sample acid peak height, mm;
h.——standard sample acid peak height, mm
m——acid mass, g;
acid content (coupling value), %.
4.3.9 Allowable difference
E,·hX1000
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of di-J acid content
4.4.1 Summary of method
Same as 4.3.1.
4.4.2 Instruments and reagents
Di-J acid: see Appendix A for purification method.
Other conditions are the same as 4.3.2 and 4.3.3.
4.4.3 Chromatographic conditions
Mobile phase: n-propanol decahydrate tetradecamethylammonium bromide = 12+88+0.3. (5)
Other conditions are the same as 4.3.4.
4.4.4 Preparation of standard solution
HG2075-91
Weigh 0.0200g of refined di-J acid (100% di-J acid) in a 100mL beaker, add a small amount of water, dissolve with (1+4) ammonia water, adjust the pH to about 6.8 with (1+17) hydrochloric acid, dilute with water to a 100mL brown volumetric flask, shake well, and store in a dark place. Pipette 0.5, 1.0, 1.5, and 2.0mL of the above solution into 10mL brown volumetric flasks, dilute to the scale with mobile phase, and shake well. The concentrations are 0.001%, 0.002%, 0.003%, and 0.004% (m/m), respectively. The storage method is the same as 4.3.5.
4.4.5 Analysis steps
The same as 4.3.6.
4.4.6 Quantitative method
Same as 4.3.7.
Figure 2 Liquid chromatography of amino acid plus diamino acid
1 Amino amino acid; 2-amino acid; 3-diamino acid
4.4.7 Calculation of analysis results
Same as 4.3.8.
4.4.8 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.1%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
5.1 Amino acids shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that all amino acids shipped out of the factory meet the requirements of this standard. Each batch of amino acids shipped out of the factory shall be accompanied by a quality certificate in a certain format. 5.2 Diamino acid is a random inspection item, and random inspection shall be carried out at least once a week. 6
HG207591
5.3 The user shall conduct quality inspection on the received J acid in accordance with the provisions of this standard to check wh
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