GB/T 5009.29-2003 Determination of sorbic acid and benzoic acid in foods
Some standard content:
National Standard of the People's Republic of China
GB/T 5009.29--2003
Replaced by CB/T=0c9.23-1996
Determinition of sorbir: acid and benzioe acid in foods
Determinition of sorbir: acid and benzioe acid in foods2003-08-11Published
Ministry of Health of the People's Republic of China
China National Standardization Administration
2004-01-01Implementation
GB/T 5009.29--2003
This standard replaces (T5009.2915S Sorbic acid in food). Compared with GB/T5009.2-1906, the main changes in this standard are as follows: 1. The Chinese name of the standard is modified. The Chinese name of the standard is changed to Sorbic acid in food. Determination of hydroxyl radicals 3; 3. The original standard structure is carried out in accordance with (B/T20001.4-2001 Standard Writing Rules Part 4, Chemical Analysis Method 3) and approved by the Ministry of Health of the People's Republic of China for import and export and unified. This standard is issued by the Ministry of Health of the People's Republic of China, and the Lanzhou Supervision and Inspection Institute is responsible for drafting this standard. This standard was drafted by Tianxiang Food Hygiene Inspection Institute, Binhsiang Food Hygiene Inspection Institute, Wuhan Sanitary and Epidemic Prevention Station, Zhejiang Provincial Epidemic Prevention Station, and Xichuan Provincial Health Prevention Station. The first draft of this standard was drafted by the Ministry of Food Hygiene Inspection Institute. This standard was first issued in 1985 and implemented for the first time in 1990. This is the second revision. 232
1 Standard
Determination of sorbic acid and malic acid in foods
This standard specifies the determination method of sorbic acid and malic acid in foods such as oil, iced fruit juice, etc. This standard is applicable to the determination of sorbic acid and malic acid in foods such as soy sauce, fruit juice, etc. GB/T 5009.29-2003
Lower detection limit: The lower detection limit is 1. When the sample used for colorimetric analysis is 1*, the maximum detection limit is 1 tg/kg
Method 1 Gas chromatography
2 Principle
After the sample is acidified, acetaldehyde is used to extract behenic acid and formic acid. The sample is separated and determined by a gas chromatograph with a ionization detector. The sample is quantitatively compared with the standard series.
3 Reagents
3.1 Acetaldehyde: not peroxide.
3.2 Non-oleic aldehydes have a boiling range of 0.~i.
3.3 Salt,
3.4 Sodium sulfate
3.5 Salt (1+1) Collect 1L hydrochloric acid and dilute to 2KmL with water.3.6 Sodium oxide acid solution (4 0%/), add a small amount of hydrochloric acid 1+1) to the oxidized caustic soda (<10%/1), acidify, 3.7.Benzene standard solution: accurately weigh more than 0.2000 of each material, place in a 100mL volumetric flask, use a non-oily-acetaldehyde (3+1) solvent and dissolve until it is dissolved, add 2 ml of single or medium acid, 3.B.sorbic acid, acetic acid standard solution: absorb appropriate amount of chrysanthemum type, benzene standard solution, dilute the sample with petroleum ether-acetaldehyde (3+1] mixed solvent equivalent to 53, 100, 150.200, 25℃ sorbic acid or benzoic acid per ml. 4. The gas chromatograph was tested by a hydrogen flame ionizer. The results were shown in step 5.1. Sample extraction. Weigh 2.50 samples mixed evenly in advance, add 10 ml of hydrochloric acid (1+1) to 8% m/s, and extract with 1510 ml of acetaldehyde. Heat for three minutes, pour the upper 7.0 ml extract into another 25 ml filter, and combine the acetaldehyde extract. Wash twice with 40 L of sodium ion solution, and pour the lower layer into a 2 ml volumetric medium with a 10 ml dropper. Add acetaldehyde to the mark, and accurately draw 5ml. Take the acetaldehyde and filter it into a 400-1000m2 test tube with a scale, place it on a 400-1000m2 water plate, add 2-acetyl condensate (3-2) to mix the mixture and set aside. 233
GB/T5009.292003
5.2 Chromatographic reference inserts
5.2.1 Chromatographic column: glass ±, inner diameter 3mm, length 2m, internal type is fixed with 5% 13CS-% zirconium acid for 60-8 days.
5.2.2 Gas flow rate, carrier The gas is oxygen, 5VmL/miu (hydrogen is air, the ratio of hydrogen to each instrument model is not selected. The optimal ratio conditions are as follows:
5.2.3 Temperature: inlet 20%℃, detector 230%, column 170℃, 5.3 Determination
The sample is placed in the gas chromatograph with the standard liquid of each concentration in the standard series, and the peak heights of different concentrations of sorbic acid and aldehyde can be measured. The liquid concentration is used as the standard, and the corresponding amplitude height is used as the standard to prepare the standard curve. The sample can be added at a rate of 2 seconds to measure the peak height and compare it with the standard practice order 5. 4 Calculation of results
The content of acetic acid or benzoic acid in the sample is calculated according to formula (7). AX1000
m×25×V
Wherein:
The content of acetic acid or benzoic acid in the test sample, in grams per kilogram/kg);
The mass of acetic acid or acetaldehyde in the test sample, in micrograms (μg):
The volume of the sample passing through at a certain time, in micrograms; m-the mass of the sample, in grams (g);
The volume of acetaldehyde extract absorbed at a certain time, in milliliters (mL); 5
5——The total volume of acetaldehyde extract of the sample, in milliliters (ml). The amount of acetaldehyde is multiplied by 1.13, which is the amount of sodium benzoate in the sample. The calculation result should retain two significant digits.
5.5 Precision
The absolute value of the two Schwendt determination results obtained under the more sensitive conditions is not more than 1G of the average value. 5.6 Others
The gas chromatogram of sorbic acid and formic acid is shown in Figure 1. The retention time of sorbic acid is 2min53s; the retention time of formic acid is mins24
6 Principle
The second method is high performance liquid chromatography
GH/T 5009.29—2003
The mixture is heated to remove carbon monoxide and ethanol, and then the mixture is heated to near neutrality and then fed into a high performance liquid chromatography instrument. After reverse phase chromatography separation, the properties are qualitatively and quantitatively determined according to the release time and peak surface. 7 Reagents
The reagents used in the method are analytical pure unless otherwise specified. Water is distilled water or water of equal purity. 7.1 Methanol is filtered through a concentrated membrane (U.5[m).
7.2 Dilute ammonia water (+1): Mix ammonia water and water.7.3 Acetic acid solution (0.20l/): Weigh 1.54 acetic acid with water to 1000mL. Dissolve through 0.45m core membrane.7.4 Monooxygen reduction solution (206/): Weigh 25 sodium bicarbonate (super pure). Add water to 0mL and vibrate to dissolve. 7.5 Formic acid standard stock solution: Accurately weigh 111 sodium monoammonium benzoate solution (20R/1.75r:1), heat and decompose, put it into a 155ml bottle, add water to make up to 13mL, the formic acid content is 1mg/ml as the service solution: 7.6 Accurately take 130g of benzoic acid, add sodium bicarbonate solution (2>5mL), heat and decompose, weigh it into a 11mL bottle, add water to make up to 11mL: the formic acid content is 1mg]. As the reserve tank solution: 7.7 Formic acid, Take the mixed liquid, take 12.5g of formic acid and 1.2g of sodium hyaluronate in a 100-volume bottle, add water to the mark. The sugar content in this solution is 0.1mg/m, and it is measured by 0.45m membrane method (GB/T5000.28-2003+13.4g of sodium hyaluronate can be added when measuring the fine hook). Obtain the solution by high efficiency chromatograph (chemical detector). 9 Analysis steps
9.1 Sample preparation
9.1.1 Technique: Take 1.30~10.1g of sample, put it into a small flask, stir it gently to remove the disulfide, and use water (1:1 pH 7. Add water to 10ml~20ml. Pass the membrane IIA 0.45μm), 9.1.2 Fruit juices, weigh 5.00-10.0g of sample, add water (1+1> to adjust the pH to about 7, Add water to a suitable volume, centrifuge and precipitate, filter the supernatant through a 0.45a membrane. 9.1.3 Prepare alcoholic beverages, weigh 10.) sample, put it into a small cup, add water to a suitable volume, add 7.5% alcohol, and measure the pH value (1-1). Add water to a suitable volume, filter through a 15m filter. 9.2 High performance liquid chromatography, please refer to the conditions of 9.2.1#: YwC4.$mmx200mm.1umm stainless steel. 9.2.2 Mobile phase, aldehyde: ethyl acetate (9.02mnl/T) (5195): 9.2.3 Di: 1 ml./mim.
9.2.4 Sample injection: 13 μL,
9.2.5 Detector: UV detector, 230nm, 0.2ALFS, qualitative according to retention time, quantitative according to external standard area. 9.3 The content of lysine or hydroxyl in the sample is calculated according to formula (2): x =
Wu Zhong:
A ×1
×1000
Content of benzoic acid or benzyl alcohol in the sample, in grams per kilogram (g/kg); Content of benzoic acid or benzyl alcohol in the sample volume, in grams (g); Sample volume, in milliliters (m3);
Total volume of the sample, in liters (l111).2 Sample mass, in grams (8);
The calculation result shall retain two significant digits.
a.4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic half mean. 9.5 Others
Same as 5.6 of R/T5005.29-2003:
In: This method can be used to determine the content of sodium in two ways. Method 3 Thin screen chromatography
10 Principle
After the sample is acidified, acetaldehyde is used to extract formic acid and sorbic acid. The sample extract is concentrated and spotted on a polyamide thin layer plate. After color development, the ratio of formic acid and sorbic acid on the thin layer plate is compared with the standard for qualitative analysis, and quantitative analysis can be performed. 236
11 Reagents
11.1 Isopropylamine.
11.2 n-Butyl alcohol
11.3 petroleum ether: boiling range 3c℃~60℃
1F.47: does not contain peroxide,
11.5 effective water.
11.6 anhydrous ethanol,
11.7 polyamide powder: 200 liters.
13.8 salt (1:), take 155mL with acid, add water to dilute to 200mL GD/T 5009.292003
11.9 Sodium chloride solution (40%/1.): Add 1% hydrochloric acid (: + 1) to the sodium chloride solution (40R/1.) to acidify. 11.10 Preparation:
11.10.1 N-Hydroxyethanol + Nitrogen water - Anhydrous ethanol (71:2). 11.10.2 Isopropyl alcohol + Hydrogen water - Anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: Accurately weigh 0.20 0% single stock, add a small amount of ethanol to a 100mL volumetric flask and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of dye. 11.12 Behenic acid standard solution: Accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of benzyl alcohol. 11.13 Colorimetric test: Add 0.4% benzaldehyde to the solution (1. ). Use sodium hydroxide group (4g/L.) to adjust to pH = S12 Preparation
12.1 Blower! .
12.2 Layer folding cylinder.
12.3 Glass plate: 19am×18cml
12.4 Microinjection nozzle: 10.100.
12.5 Sprayer.
13 Analysis steps
13.1 Sample extraction
Take 2,5 0g of the first mixed sample is placed in a 25mL dense tank: add 0.51ml of hydrochloric acid (1 + 1) to acidify. Take 50L of acetaldehyde twice, add 11ml each time, and absorb the upper aldehyde into another 25mL, fill it with a dense tube, combine the ethyl acetate absorption liquid: wash off the two drinks with 4ml of chlorinated aldehyde (40Cg/L?), let it stand for 15min, and use a dropper to drain the acetaldehyde layer through anhydrous flow into a 25mL container. Add ethyl acetate to the full scale, adjust, and absorb 15.ml of acetaldehyde into 1μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1ml of appropriate solution, and set aside. 13.2 Determination
13.2.1 Preparation of powder plate: Weigh 1.6 g of acyl gelatin powder, add 0.4 g of canned powder, add about 15 ml of water, grind for 5 min~5 min, immediately put into the applicator to make two thin layer plates of 10 cm×1% cm and thickness of c,3 mm, dry at room temperature for 10 min: dry for 1 h: place in a desiccator and keep. 13.2.2 Spotting: On the baseline 2 m below the thin layer plate, use a micro-radiograph to spot 1 L and 2 L of the sample solution at the same time, and use the standard wave with facial acid and formic acid.
13.2.3 Development and color quality: Place the spotted plate in a developing solution pre-prepared with developing agent (11.1.1 or 11.10.3). Place filter paper around the developing solution and spread the front edge of the droplet to 101. Take it out and spray the color developing agent. The spots are yellow and the disk is blue. The amount of sorbic acid and benzoic acid in the sample is quantitatively compared with the standard sample (the relative values of sorbic acid and benzoic acid are 0.82 and 0.73, respectively). 2.37
CB/T5009.29--2003
13.3 Result calculation
The amount of aldehyde or sorbitan in the test sample is measured by formula (3).
mx taste * note
total!
test formic acid or sorbitan modified full point, unit is gram per kilogram [g/kA
determination of the sample in the form of formic acid mass unit is bright gram (Mg) added to the body, unit is milliliter (m) real-time sample volume. Firm position is liter (mL)! Test air volume, unit is gram (g):
timed collection of acetic acid to avoid the volume of the report, unit is liter (ml.): the sample fresh standard to provide, unit is liter (mI.). This method can also be used to determine the sample, to calculate the sample, with the anti-commercial agent qualitative test
14 Boric acid, ketoacyl
14.t Reagents
14.1.1 Boric acid (11): 100mL of sodium hydroxide, add 200mL of water..14,1.2 Magnetic acid hook (408/1.).
14.1.3 Platinum hydroxide solution (4g/I.) Take 2B sodium hydride, add water and dilute to 500mL. 14.1.4 Test paper: weigh 20% yellow potential *, wash with cold water 4 times, each time 1001r:T. After removing the water, dry the residue at T. Add 1 r. ethanol, no count, filter, take 1rmm filter paper strip, no deep reduction, take out, dry in air for ten times, glass plate
14.2 Steps
14.2.1 Sample treatment
Weigh ~ solid sample, add sodium phosphate (4% sodium carbonate) to make it moist, dry it on a low fire, carbonize it, and then put it in a high temperature furnace to heat it, and collect 101ml.-~21r:1. Liquid sample. I carbonic acid solution (106/1) until it is magnetic, then put it in a water bath to steam for ten times, and then put it in a commercial furnace to heat it
14. 2.2 Qualitative test
14.2.2.1 Differential test paper method: Take all the ash, add a small amount of this and hydrochloric acid (1-1) until it is slightly acidic, stir while dropping, make the filter paper decompose, change the temperature and drain. Put the negative test paper into the filter, take out the test paper, and keep it warm. Dry it at 60℃~7℃ for a period of time. When sand is present, the test paper shows part or all color, and the part with color turns green immediately. 14.2.2.? Color should be added: Mix the ash and add a few drops of ethanol, ignite directly, and when the acid turns green, the fire sample is green:
15 Hydrogen bridge acid
15.1 Reagents
15.1.1 Trinitride soft melt (11/1.). 15.1.2 Industrial nitric acid (.3) 1.7.
15.1.3 Ethylene (50%).
15.1.4 Pyrolysis of 102g/mol: limit 0g pyrolysis period (u, 5H0 hydrolyzed to 100258
15.2 Analysis steps
15.2.1 Sample grip
According to 3.1 of GB/TE009.28
32C3, after evaporating the acetaldehyde extract to dryness, set aside for use. 15. 2, 2 Qualitative test
GB/T 5009.29—2003
15.2.2.1 Ferric chloride method, add 1~2 drops of ferric chloride to the residual activity (:0R/1.3), and the color will be blue when salicylic acid is present. 15.2.2.2 Confirmation test: Dissolve in a small amount of hot water, cool, add 4~5 drops of sub-acid benzoate (1008/[.), 5 drops of acetic acid () and 1 drop of copper sulfate (150g/.>), drain, drain 0.5, and let stand for a while. The amount of water acid is blood red (mimicry acid is the color)1 ml./mim.
9.2.4 Injection volume: 13 μL,
9.2.5 Detector: UV detector, 230nm wavelength 0.2ALFS, qualitative analysis based on retention time, quantitative analysis based on external standard area. 9.3 Calculate the content of lycopene or lycopene in the sample according to formula (2): x=
Wu Zhong:
A ×1
×1000
Content of benzoic acid or benzyl alcohol in the sample, in grams per kilogram (g/kg); Content of benzoic acid or benzyl alcohol in the sample volume, in grams (g); Sample volume, in milliliters (m3);
Total volume of the sample, in liters (l111).2 Sample mass, in grams (8);
The calculation result shall retain two significant digits.
a.4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic half mean. 9.5 Others
Same as 5.6 of R/T5005.29-2003:
In: This method can be used to determine the content of sodium in two ways. Method 3 Thin screen chromatography
10 Principle
After the sample is acidified, acetaldehyde is used to extract formic acid and sorbic acid. The sample extract is concentrated and spotted on a polyamide thin layer plate. After color development, the ratio of formic acid and sorbic acid on the thin layer plate is compared with the standard for qualitative analysis, and quantitative analysis can be performed. 236
11 Reagents
11.1 Isopropylamine.
11.2 n-Butyl alcohol
11.3 petroleum ether: boiling range 3c℃~60℃
1F.47: does not contain peroxide,
11.5 effective water.
11.6 anhydrous ethanol,
11.7 polyamide powder: 200 liters.
13.8 salt (1:), take 155mL with acid, add water to dilute to 200mL GD/T 5009.292003
11.9 Sodium chloride solution (40%/1.): Add 1% hydrochloric acid (: + 1) to the sodium chloride solution (40R/1.) to acidify. 11.10 Preparation:
11.10.1 N-Hydroxyethanol + Nitrogen water - Anhydrous ethanol (71:2). 11.10.2 Isopropyl alcohol + Hydrogen water - Anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: Accurately weigh 0.20 0% single stock, add a small amount of ethanol to a 100mL volumetric flask and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of dye. 11.12 Behenic acid standard solution: Accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of benzyl alcohol. 11.13 Colorimetric test: Add 0.4% benzaldehyde to the solution (1. ). Use sodium hydroxide group (4g/L.) to adjust to pH = S12 Preparation
12.1 Blower! .
12.2 Layer folding cylinder.
12.3 Glass plate: 19am×18cml
12.4 Microinjection nozzle: 10.100.
12.5 Sprayer.
13 Analysis steps
13.1 Sample extraction
Take 2,5 0g of the first mixed sample is placed in a 25mL dense tank: add 0.51ml of hydrochloric acid (1 + 1) to acidify. Take 50L of acetaldehyde twice, add 11ml each time, and absorb the upper aldehyde into another 25mL, fill it with a dense tube, combine the ethyl acetate absorption liquid: wash off the two drinks with 4ml of chlorinated aldehyde (40Cg/L?), let it stand for 15min, and use a dropper to drain the acetaldehyde layer through anhydrous flow into a 25mL container. Add ethyl acetate to the full scale, adjust, and absorb 15.ml of acetaldehyde into 1μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1ml of appropriate solution, and set aside. 13.2 Determination
13.2.1 Preparation of powder plate: Weigh 1.6 g of acyl gelatin powder, add 0.4 g of canned powder, add about 15 ml of water, grind for 5 min~5 min, immediately put into the applicator to make two thin layer plates of 10 cm×1% cm and thickness of c,3 mm, dry at room temperature for 10 min: dry for 1 h: place in a desiccator and keep. 13.2.2 Spotting: On the baseline 2 m below the thin layer plate, use a micro-radiograph to spot 1 L and 2 L of the sample solution at the same time, and use the standard wave with facial acid and formic acid.
13.2.3 Development and color quality: Place the spotted plate in a developing solution pre-prepared with developing agent (11.1.1 or 11.10.3). Place filter paper around the developing solution and spread the front edge of the droplet to 101. Take it out and spray the color developing agent. The spots are yellow and the disk is blue. The amount of sorbic acid and benzoic acid in the sample is quantitatively compared with the standard sample (the relative values of sorbic acid and benzoic acid are 0.82 and 0.73, respectively). 2.37
CB/T5009.29--2003
13.3 Result calculation
The amount of aldehyde or sorbitan in the test sample is measured by formula (3).
mx taste * note
total!
test formic acid or sorbitan modified full point, unit is gram per kilogram [g/kA
determination of the sample in the form of formic acid mass unit is bright gram (Mg) added to the body, unit is milliliter (m) real-time sample volume. Firm position is liter (mL)! Test air volume, unit is gram (g):
timed collection of acetic acid to avoid the volume of the report, unit is liter (ml.): the sample fresh standard to provide, unit is liter (mI.). This method can also be used to determine the sample, to calculate the sample, with the anti-commercial agent qualitative test
14 Boric acid, ketoacyl
14.t Reagents
14.1.1 Boric acid (11): 100mL of sodium hydroxide, add 200mL of water..14,1.2 Magnetic acid hook (408/1.).
14.1.3 Platinum hydroxide solution (4g/I.) Take 2B sodium hydride, add water and dilute to 500mL. 14.1.4 Test paper: weigh 20% yellow potential *, wash with cold water 4 times, each time 1001r:T. After removing the water, dry the residue at T. Add 1 r. ethanol, no count, filter, take 1rmm filter paper strip, no deep reduction, take out, dry in air for ten times, glass plate
14.2 Steps
14.2.1 Sample treatment
Weigh ~ solid sample, add sodium phosphate (4% sodium carbonate) to make it moist, dry it on a low fire, carbonize it, and then put it in a high temperature furnace to heat it, and collect 101ml.-~21r:1. Liquid sample. I carbonic acid solution (106/1) until it is magnetic, then put it in a water bath to steam for ten times, and then put it in a commercial furnace to heat it
14. 2.2 Qualitative test
14.2.2.1 Differential test paper method: Take all the ash, add a small amount of this and hydrochloric acid (1-1) until it is slightly acidic, stir while dropping, make the filter paper decompose, change the temperature and drain. Put the negative test paper into the filter, take out the test paper, and keep it warm. Dry it at 60℃~7℃ for a period of time. When sand is present, the test paper shows part or all color, and the part with color turns green immediately. 14.2.2.? Color should be added: Mix the ash and add a few drops of ethanol, ignite directly, and when the acid turns green, the fire sample is green:
15 Hydrogen bridge acid
15.1 Reagents
15.1.1 Trinitride soft melt (11/1.). 15.1.2 Industrial nitric acid (.3) 1.7.
15.1.3 Ethylene (50%).
15.1.4 Pyrolysis of 102g/mol: limit 0g pyrolysis period (u, 5H0 hydrolyzed to 100258
15.2 Analysis steps
15.2.1 Sample grip
According to 3.1 of GB/TE009.28
32C3, after evaporating the acetaldehyde extract to dryness, set aside for use. 15. 2, 2 Qualitative test
GB/T 5009.29—2003
15.2.2.1 Ferric chloride method, add 1~2 drops of ferric chloride to the residual activity (:0R/1.3), and the color will be blue when salicylic acid is present. 15.2.2.2 Confirmation test: Dissolve in a small amount of hot water, cool, add 4~5 drops of sub-acid benzoate (1008/[.), 5 drops of acetic acid () and 1 drop of copper sulfate (150g/.>), drain, drain 0.5, and let stand for a while. The amount of water acid is blood red (mimicry acid is the color)1 ml./mim.
9.2.4 Injection volume: 13 μL,
9.2.5 Detector: UV detector, 230nm wavelength 0.2ALFS, qualitative analysis based on retention time, quantitative analysis based on external standard area. 9.3 Calculate the content of lycopene or lycopene in the sample according to formula (2): x=
Wu Zhong:
A ×1
×1000
Content of benzoic acid or benzyl alcohol in the sample, in grams per kilogram (g/kg); Content of benzoic acid or benzyl alcohol in the sample volume, in grams (g); Sample volume, in milliliters (m3);
Total volume of the sample, in liters (l111).2 Sample mass, in grams (8);
The calculation result shall retain two significant digits.
a.4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic half mean. 9.5 Others
Same as 5.6 of R/T5005.29-2003:
In: This method can be used to determine the content of sodium in two ways. Method 3 Thin screen chromatography
10 Principle
After the sample is acidified, acetaldehyde is used to extract formic acid and sorbic acid. The sample extract is concentrated and spotted on a polyamide thin layer plate. After color development, the ratio of formic acid and sorbic acid on the thin layer plate is compared with the standard for qualitative analysis, and quantitative analysis can be performed. 236
11 Reagents
11.1 Isopropylamine.
11.2 n-Butyl alcohol
11.3 petroleum ether: boiling range 3c℃~60℃
1F.47: does not contain peroxide,
11.5 effective water.
11.6 anhydrous ethanol,
11.7 polyamide powder: 200 liters.
13.8 salt (1:), take 155mL with acid, add water to dilute to 200mL GD/T 5009.292003
11.9 Sodium chloride solution (40%/1.): Add 1% hydrochloric acid (: + 1) to the sodium chloride solution (40R/1.) to acidify. 11.10 Preparation:
11.10.1 N-Hydroxyethanol + Nitrogen water - Anhydrous ethanol (71:2). 11.10.2 Isopropyl alcohol + Hydrogen water - Anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: Accurately weigh 0.20 0% single stock, add a small amount of ethanol to a 100mL volumetric flask and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of dye. 11.12 Behenic acid standard solution: Accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of benzyl alcohol. 11.13 Colorimetric test: Add 0.4% benzaldehyde to the solution (1. ). Use sodium hydroxide group (4g/L.) to adjust to pH = S12 Preparation
12.1 Blower! .
12.2 Layer folding cylinder.
12.3 Glass plate: 19am×18cml
12.4 Microinjection nozzle: 10.100.
12.5 Sprayer.
13 Analysis steps
13.1 Sample extraction
Take 2,5 0g of the first mixed sample is placed in a 25mL dense tank: add 0.51ml of hydrochloric acid (1 + 1) to acidify. Take 50L of acetaldehyde twice, add 11ml each time, and absorb the upper aldehyde into another 25mL, fill it with a dense tube, combine the ethyl acetate absorption liquid: wash off the two drinks with 4ml of chlorinated aldehyde (40Cg/L?), let it stand for 15min, and use a dropper to drain the acetaldehyde layer through anhydrous flow into a 25mL container. Add ethyl acetate to the full scale, adjust, and absorb 15.ml of acetaldehyde into 1μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1ml of appropriate solution, and set aside. 13.2 Determination
13.2.1 Preparation of powder plate: Weigh 1.6 g of acyl gelatin powder, add 0.4 g of canned powder, add about 15 ml of water, grind for 5 min~5 min, immediately put into the applicator to make two thin layer plates of 10 cm×1% cm and thickness of c,3 mm, dry at room temperature for 10 min: dry for 1 h: place in a desiccator and keep. 13.2.2 Spotting: On the baseline 2 m below the thin layer plate, use a micro-radiograph to spot 1 L and 2 L of the sample solution at the same time, and use the standard wave with facial acid and formic acid.
13.2.3 Development and color quality: Place the spotted plate in a developing solution pre-prepared with developing agent (11.1.1 or 11.10.3). Place filter paper around the developing solution and spread the front edge of the droplet to 101. Take it out and spray the color developing agent. The spots are yellow and the disk is blue. The amount of sorbic acid and benzoic acid in the sample is quantitatively compared with the standard sample (the relative values of sorbic acid and benzoic acid are 0.82 and 0.73, respectively). 2.37
CB/T5009.29--2003
13.3 Result calculation
The amount of aldehyde or sorbitan in the test sample is measured by formula (3).
mx taste * note
total!
test formic acid or sorbitan modified full point, unit is gram per kilogram [g/kA
determination of the sample in the form of formic acid mass unit is bright gram (Mg) added to the body, unit is milliliter (m) real-time sample volume. Firm position is liter (mL)! Test air volume, unit is gram (g):
timed collection of acetic acid to avoid the volume of the report, unit is liter (ml.): the sample fresh standard to provide, unit is liter (mI.). This method can also be used to determine the sample, to calculate the sample, with the anti-commercial agent qualitative test
14 Boric acid, ketoacyl
14.t Reagents
14.1.1 Boric acid (11): 100mL of sodium hydroxide, add 200mL of water..14,1.2 Magnetic acid hook (408/1.).
14.1.3 Platinum hydroxide solution (4g/I.) Take 2B sodium hydride, add water and dilute to 500mL. 14.1.4 Test paper: weigh 20% yellow potential *, wash with cold water 4 times, each time 1001r:T. After removing the water, dry the residue at T. Add 1 r. ethanol, no count, filter, take 1rmm filter paper strip, no deep reduction, take out, dry in air for ten times, glass plate
14.2 Steps
14.2.1 Sample treatment
Weigh ~ solid sample, add sodium phosphate (4% sodium carbonate) to make it moist, dry it on a low fire, carbonize it, and then put it in a high temperature furnace to heat it, and collect 101ml.-~21r:1. Liquid sample. I carbonic acid solution (106/1) until it is magnetic, then put it in a water bath to steam for ten times, and then put it in a commercial furnace to heat it
14. 2.2 Qualitative test
14.2.2.1 Differential test paper method: Take all the ash, add a small amount of this and hydrochloric acid (1-1) until it is slightly acidic, stir while dropping, make the filter paper decompose, change the temperature and drain. Put the negative test paper into the filter, take out the test paper, and keep it warm. Dry it at 60℃~7℃ for a period of time. When sand is present, the test paper shows part or all color, and the part with color turns green immediately. 14.2.2.? Color should be added: Mix the ash and add a few drops of ethanol, ignite directly, and when the acid turns green, the fire sample is green:
15 Hydrogen bridge acid
15.1 Reagents
15.1.1 Trinitride soft melt (11/1.). 15.1.2 Industrial nitric acid (.3) 1.7.
15.1.3 Ethylene (50%).
15.1.4 Pyrolysis of 102g/mol: limit 0g pyrolysis period (u, 5H0 hydrolyzed to 100258
15.2 Analysis steps
15.2.1 Sample grip
According to 3.1 of GB/TE009.28
32C3, after evaporating the acetaldehyde extract to dryness, set aside for use. 15. 2, 2 Qualitative test
GB/T 5009.29—2003
15.2.2.1 Ferric chloride method, add 1~2 drops of ferric chloride to the residual activity (:0R/1.3), and the color will be blue when salicylic acid is present. 15.2.2.2 Confirmation test: Dissolve in a small amount of hot water, cool, add 4~5 drops of sub-acid benzoate (1008/[.), 5 drops of acetic acid () and 1 drop of copper sulfate (150g/.>), drain, drain 0.5, and let stand for a while. The amount of water acid is blood red (mimicry acid is the color)3 The content of benzoic acid or benzyl alcohol in the sample shall be calculated according to formula (2): x=
Where:
A×1
×1000
The content of benzoic acid or benzyl alcohol in the sample, in grams per kilogram (g/kg); The content of benzoic acid or benzyl alcohol in the sample, in grams (g); The sample volume, in milliliters (m2); The total volume of the sample, in milliliters (lml); The mass of the sample, in grams (8); The calculation result shall retain two valid digits.
A.4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic half mean. 9.5 Others
Same as 5.6 of R/T5005.29-2003:
In: This method can be used to determine the content of sodium in two ways. Method 3 Thin screen chromatography
10 Principle
After the sample is acidified, acetaldehyde is used to extract formic acid and sorbic acid. The sample extract is concentrated and spotted on a polyamide thin layer plate. After color development, the ratio of formic acid and sorbic acid on the thin layer plate is compared with the standard for qualitative analysis, and quantitative analysis can be performed. 236
11 Reagents
11.1 Isopropylamine.
11.2 n-Butyl alcohol
11.3 petroleum ether: boiling range 3c℃~60℃
1F.47: does not contain peroxide,
11.5 effective water.
11.6 anhydrous ethanol,
11.7 polyamide powder: 200 liters.
13.8 salt (1:), take 155mL with acid, add water to dilute to 200mL GD/T 5009.292003
11.9 Sodium chloride solution (40%/1.): Add 1% hydrochloric acid (: + 1) to the sodium chloride solution (40R/1.) to acidify. 11.10 Preparation:
11.10.1 N-Hydroxyethanol + Nitrogen water - Anhydrous ethanol (71:2). 11.10.2 Isopropyl alcohol + Hydrogen water - Anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: Accurately weigh 0.20 0% single stock, add a small amount of ethanol to a 100mL volumetric flask and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of dye. 11.12 Behenic acid standard solution: Accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of benzyl alcohol. 11.13 Colorimetric test: Add 0.4% benzaldehyde to the solution (1. ). Use sodium hydroxide group (4g/L.) to adjust to pH = S12 Preparation
12.1 Blower! .
12.2 Layer folding cylinder.
12.3 Glass plate: 19am×18cml
12.4 Microinjection nozzle: 10.100.
12.5 Sprayer.
13 Analysis steps
13.1 Sample extraction
Take 2,5 0g of the first mixed sample is placed in a 25mL dense tank: add 0.51ml of hydrochloric acid (1 + 1) to acidify. Take 50L of acetaldehyde twice, add 11ml each time, and absorb the upper aldehyde into another 25mL, fill it with a dense tube, combine the ethyl acetate absorption liquid: wash off the two drinks with 4ml of chlorinated aldehyde (40Cg/L?), let it stand for 15min, and use a dropper to drain the acetaldehyde layer through anhydrous flow into a 25mL container. Add ethyl acetate to the full scale, adjust, and absorb 15.ml of acetaldehyde into 1μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1ml of appropriate solution, and set aside. 13.2 Determination
13.2.1 Preparation of powder plate: Weigh 1.6 g of acyl gelatin powder, add 0.4 g of canned powder, add about 15 ml of water, grind for 5 min~5 min, immediately put into the applicator to make two thin layer plates of 10 cm×1% cm and thickness of c,3 mm, dry at room temperature for 10 min: dry for 1 h: place in a desiccator and keep. 13.2.2 Spotting: On the baseline 2 m below the thin layer plate, use a micro-radiograph to spot 1 L and 2 L of the sample solution at the same time, and use the standard wave with facial acid and formic acid.
13.2.3 Development and color quality: Place the spotted plate in a developing solution pre-prepared with developing agent (11.1.1 or 11.10.3). Place filter paper around the developing solution and spread the front edge of the droplet to 101. Take it out and spray the color developing agent. The spots are yellow and the disk is blue. The amount of sorbic acid and benzoic acid in the sample is quantitatively compared with the standard sample (the relative values of sorbic acid and benzoic acid are 0.82 and 0.73, respectively). 2.37
CB/T5009.29--2003
13.3 Result calculation
The amount of aldehyde or sorbitan in the test sample is measured by formula (3).
mx taste * note
total!
test formic acid or sorbitan modified full point, unit is gram per kilogram [g/kA
determination of the sample in the form of formic acid mass unit is bright gram (Mg) added to the body, unit is milliliter (m) real-time sample volume. Firm position is liter (mL)! Test air volume, unit is gram (g):
timed collection of acetic acid to avoid the volume of the report, unit is liter (ml.): the sample fresh standard to provide, unit is liter (mI.). This method can also be used to determine the sample, to calculate the sample, with the anti-commercial agent qualitative test
14 Boric acid, ketoacyl
14.t Reagents
14.1.1 Boric acid (11): 100mL of sodium hydroxide, add 200mL of water..14,1.2 Magnetic acid hook (408/1.).
14.1.3 Platinum hydroxide solution (4g/I.) Take 2B sodium hydride, add water and dilute to 500mL. 14.1.4 Test paper: weigh 20% yellow potential *, wash with cold water 4 times, each time 1001r:T. After removing the water, dry the residue at T. Add 1 r. ethanol, no count, filter, take 1rmm filter paper strip, no deep reduction, take out, dry in air for ten times, glass plate
14.2 Steps
14.2.1 Sample treatment
Weigh ~ solid sample, add sodium phosphate (4% sodium carbonate) to make it moist, dry it on a low fire, carbonize it, and then put it in a high temperature furnace to heat it, and collect 101ml.-~21r:1. Liquid sample. I carbonic acid solution (106/1) until it is magnetic, then put it in a water bath to steam for ten times, and then put it in a commercial furnace to heat it
14. 2.2 Qualitative test
14.2.2.1 Differential test paper method: Take all the ash, add a small amount of this and hydrochloric acid (1-1) until it is slightly acidic, stir while dropping, make the filter paper decompose, change the temperature and drain. Put the negative test paper into the filter, take out the test paper, and keep it warm. Dry it at 60℃~7℃ for a period of time. When sand is present, the test paper shows part or all color, and the part with color turns green immediately. 14.2.2.? Color should be added: Mix the ash and add a few drops of ethanol, ignite directly, and when the acid turns green, the fire sample is green:
15 Hydrogen bridge acid
15.1 Reagents
15.1.1 Trinitride soft melt (11/1.). 15.1.2 Industrial nitric acid (.3) 1.7.
15.1.3 Ethylene (50%).
15.1.4 Pyrolysis of 102g/mol: limit 0g pyrolysis period (u, 5H0 hydrolyzed to 100258
15.2 Analysis steps
15.2.1 Sample grip
According to 3.1 of GB/TE009.28
32C3, after evaporating the acetaldehyde extract to dryness, set aside for use. 15. 2, 2 Qualitative test
GB/T 5009.29—2003
15.2.2.1 Ferric chloride method, add 1~2 drops of ferric chloride to the residual activity (:0R/1.3), and the color will be blue when salicylic acid is present. 15.2.2.2 Confirmation test: Dissolve in a small amount of hot water, cool, add 4~5 drops of sub-acid benzoate (1008/[.), 5 drops of acetic acid () and 1 drop of copper sulfate (150g/.>), drain, drain 0.5, and let stand for a while. The amount of water acid is blood red (mimicry acid is the color)3 The content of benzoic acid or benzyl alcohol in the sample shall be calculated according to formula (2): x=
Where:
A×1
×1000
The content of benzoic acid or benzyl alcohol in the sample, in grams per kilogram (g/kg); The content of benzoic acid or benzyl alcohol in the sample, in grams (g); The sample volume, in milliliters (m2); The total volume of the sample, in milliliters (lml); The mass of the sample, in grams (8); The calculation result shall retain two valid digits.
A.4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic half mean. 9.5 Others
Same as 5.6 of R/T5005.29-2003:
In: This method can be used to determine the content of sodium in two ways. Method 3 Thin screen chromatography
10 Principle
After the sample is acidified, acetaldehyde is used to extract formic acid and sorbic acid. The sample extract is concentrated and spotted on a polyamide thin layer plate. After color development, the ratio of formic acid and sorbic acid on the thin layer plate is compared with the standard for qualitative analysis, and quantitative analysis can be performed. 236
11 Reagents
11.1 Isopropylamine.
11.2 n-Butyl alcohol
11.3 petroleum ether: boiling range 3c℃~60℃
1F.47: does not contain peroxide,
11.5 effective water.
11.6 anhydrous ethanol,
11.7 polyamide powder: 200 liters.
13.8 salt (1:), take 155mL with acid, add water to dilute to 200mL GD/T 5009.292003
11.9 Sodium chloride solution (40%/1.): Add 1% hydrochloric acid (: + 1) to the sodium chloride solution (40R/1.) to acidify. 11.10 Preparation:
11.10.1 N-Hydroxyethanol + Nitrogen water - Anhydrous ethanol (71:2). 11.10.2 Isopropyl alcohol + Hydrogen water - Anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: Accurately weigh 0.20 0% single stock, add a small amount of ethanol to a 100mL volumetric flask and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of dye. 11.12 Behenic acid standard solution: Accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0mg of benzyl alcohol. 11.13 Colorimetric test: Add 0.4% benzaldehyde to the solution (1. ). Use sodium hydroxide group (4g/L.) to adjust to pH = S12 Preparation
12.1 Blower! .
12.2 Layer folding cylinder.
12.3 Glass plate: 19am×18cml
12.4 Microinjection nozzle: 10.100.
12.5 Sprayer.
13 Analysis steps
13.1 Sample extraction
Take 2,5 0g of the first mixed sample is placed in a 25mL dense tank: add 0.51ml of hydrochloric acid (1 + 1) to acidify. Take 50L of acetaldehyde twice, add 11ml each time, and absorb the upper aldehyde into another 25mL, fill it with a dense tube, combine the ethyl acetate absorption liquid: wash off the two drinks with 4ml of chlorinated aldehyde (40Cg/L?), let it stand for 15min, and use a dropper to drain the acetaldehyde layer through anhydrous flow into a 25mL container. Add ethyl acetate to the full scale, adjust, and absorb 15.ml of acetaldehyde into 1μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1ml of appropriate solution, and set aside. 13.2 Determination
13.2.1 Preparation of powder plate: Weigh 1.6 g of acyl gelatin powder, add 0.4 g of canned powder, add about 15 ml of water, grind for 5 min~5 min, immediately put into the applicator to make two thin layer plates of 10 cm×1% cm and thickness of c,3 mm, dry at room temperature for 10 min: dry for 1 h: place in a desiccator and keep. 13.2.2 Spotting: On the baseline 2 m below the thin layer plate, use a micro-radiograph to spot 1 L and 2 L of the sample solution at the same time, and use the standard wave with facial acid and formic acid.
13.2.3 Development and color quality: Place the spotted plate in a developing solution pre-prepared with developing agent (11.1.1 or 11.10.3). Place filter paper around the developing solution and spread the front edge of the droplet to 101. Take it out and spray the color developing agent. The spots are yellow and the disk is blue. The amount of sorbic acid and benzoic acid in the sample is quantitatively compared with the standard sample (the relative values of sorbic acid and benzoic acid are 0.82 and 0.73, respectively). 2.37
CB/T5009.29--2003
13.3 Result calculation
The amount of aldehyde or sorbitan in the test sample is measured by formula (3).
mx taste * note
total!
test formic acid or sorbitan modified full point, unit is gram per kilogram [g/kA
determination of the sample in the form of formic acid mass unit is bright gram (Mg) added to the body, unit is milliliter (m) real-time sample volume. Firm position is liter (mL)! Test air volume, unit is gram (g):
timed collection of acetic acid to avoid the volume of the report, unit is liter (ml.): the sample fresh standard to provide, unit is liter (mI.). This method can also be used to determine the sample, to calculate the sample, with the anti-commercial agent qualitative test
14 Boric acid, ketoacyl
14.t Reagents
14.1.1 Boric acid (11): 100mL of sodium hydroxide, add 200mL of water..14,1.2 Magnetic acid hook (408/1.).
14.1.3 Platinum hydroxide solution (4g/I.) Take 2B sodium hydride, add water and dilute to 500mL. 14.1.4 Test paper: weigh 20% yellow potential *, wash with cold water 4 times, each time 1001r:T. After removing the water, dry the residue at T. Add 1 r. ethanol, no count, filter, take 1rmm filter paper strip, no deep reduction, take out, dry in air for ten times, glass plate
14.2 Steps
14.2.1 Sample treatment
Weigh ~ solid sample, add sodium phosphate (4% sodium carbonate) to make it moist, dry it on a low fire, carbonize it, and then put it in a high temperature furnace to heat it, and collect 101ml.-~21r:1. Liquid sample. I carbonic acid solution (106/1) until it is magnetic, then put it in a water bath to steam for ten times, and then put it in a commercial furnace to heat it
14. 2.2 Qualitative test
14.2.2.1 Differential test paper method: Take all the ash, add a small amount of this and hydrochloric acid (1-1) until it is slightly acidic, stir while dropping, make the filter paper decompose, change the temperature and drain. Put the negative test paper into the filter, take out the test paper, and keep it warm. Dry it at 60℃~7℃ for a period of time. When sand is present, the test paper shows part or all color, and the part with color turns green immediately. 14.2.2.? Color should be added: Mix the ash and add a few drops of ethanol, ignite directly, and when the acid turns green, the fire sample is green:
15 Hydrogen bridge acid
15.1 Reagents
15.1.1 Trinitride soft melt (11/1.). 15.1.2 Industrial nitric acid (.3) 1.7.
15.1.3 Ethylene (50%).
15.1.4 Pyrolysis of 102g/mol: limit 0g pyrolysis period (u, 5H0 hydrolyzed to 100258
15.2 Analysis steps
15.2.1 Sample grip
According to 3.1 of GB/TE009.28
32C3, after evaporating the acetaldehyde extract to dryness, set aside for use. 15. 2, 2 Qualitative test
GB/T 5009.29—2003
15.2.2.1 Ferric chloride method, add 1~2 drops of ferric chloride to the residual activity (:0R/1.3), and the color will be blue when salicylic acid is present. 15.2.2.2 Confirmation test: Dissolve in a small amount of hot water, cool, add 4~5 drops of sub-acid benzoate (1008/[.), 5 drops of acetic acid () and 1 drop of copper sulfate (150g/.>), drain, drain 0.5, and let stand for a while. The amount of water acid is blood red (mimicry acid is the color)4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic half mean. 9.5 Others
Same as 5.6 of R/T5005.29-2003:
In: The third method is thin screen chromatography
10 Principle
After the sample is acidified, formic acid and sorbic acid are extracted with acetaldehyde. The sample extract is concentrated and spotted on a polyamide thin layer plate, opened, and after color development, the ratio of formic acid and sorbic acid on the thin layer plate is compared with the standard for qualitative analysis, and quantitative analysis can be performed. 236
11 Reagents
11.1 Isopropylamine sequence.
11.2 n-butyl alcohol
11.3 petroleum ether: boiling range 3c℃~60℃
1F.47: does not contain peroxide,
11.5 effective water.
11.6 anhydrous ethanol,
11.7 polyamide rubber powder: 200 liters.
13.8 Salt (1:), take 155mL with acid, add water to dilute to 200mL GD/T 5009.292003
11.9 Sodium chloride soluble alone (40%/1.): add 1% hydrochloric acid (:+1) to the sodium chloride filter (40R/1.) to acidify 11.10 Expand the following:
11.10.1 n-T alcohol + nitrogen water-anhydrous ethyl alcohol (71:2).11.10.2 isopropyl alcohol + hydrogen water-anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: accurately weigh 0.200% benzyl alcohol, dissolve it with a small amount of ethanol and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0 mg benzyl alcohol. 11.12 Standard solution of benzyl alcohol: accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0 mg benzyl alcohol. 11.13 Colorimetric test: 1% benzyl alcohol (in%) solution (0.4%/1 mL). Adjust to pH = 5 with sodium hydroxide solution (4 g/L). Preparation
12.1 Blow dryer!
12.2 Layer folding cylinder
12.3 Glass plate: 19am×18cm
12.4 Microinjection 10.100.
12.5 Sprayer.bzxZ.net
13 Analysis Steps
13.1 Sample Extraction
Take 2.50 g of the first mixed sample and place it in a 25 mL dense tube: add 0.51 ml of hydrochloric acid (1 + 1) to acidify. Take 50 L of acetaldehyde twice, add 11 ml each time, and absorb the upper aldehyde into another 25 mL, fill the tube with dense filling, combine the acetaldehyde absorption liquid: wash the two drinks with 4 ml of chlorinated aldehyde (400 g/L), let it stand for 15 min, and use a dropper to filter the acetaldehyde layer through anhydrous flow to drain into a 25 mL container. Add acetaldehyde to the full scale, adjust, and absorb 15 ml of acetaldehyde into 1 μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1 centrifuge tubes m containing 1L of sample solution, set aside. 13.2 Determination
13.2.1 Preparation of sample powder plate: weigh 1.6g of acyl gelatin powder, add 0.4g of acetyl gelatin powder, add about 15ml of water, grind for 5min~5min, immediately put into the applicator to prepare two thin layer plates with a section of 10cm×1%cm and a thickness of c.3mm, dry at room temperature for 10min: dry for 1 hour: put in a dryer and keep. 13.2.2 Spotting: on the baseline 2m below the bottom of the thin layer plate, use a micro-radiograph to spot 1L and 2L of sample solution at the same time, and use 1L of the standard for acetic acid and formic acid.
13.2.3 Development and color matching: put the spotted plate into a developing solution pre-prepared with a developing agent (11.1.1 or 11.10.3). The filter paper around the developing area will remove the developing agent. The front edge is extended to 101 and then taken out of the turbidity. The color developer is sprayed, and the spots are yellow and the disk is blue. The amount of sorbic acid and benzoic acid contained in the material is compared with the standard point quantitatively (the specific values of sorbic acid and benzoic acid are 0.82 and 0.73 respectively). 2.37
CB/T5009.29--2003
13.3 Calculation
The total amount of sorbic acid or sorbitan in the test sample is measured by formula (3). X
mx is recorded in total!
The total amount of sorbitan in the test sample is in grams per kilogram [g/kA
The unit of the mass of the sorbitan in the test sample is bright grams (Mg) and the unit of the added sample is milliliters (m). The volume of the sample is measured in liters (mL)! Test air volume, unit is gram (g):
Timed strong collection of ethyl acetate to avoid the use of the report, unit is liter (ml.): The fresh sample is taken as described in the total supply, unit is liter (mI.). This method can also be used with the same method to determine the sample, to calculate the situation, use the commercial agent for qualitative test
14 Boric acid, ketoacyl
14.t Reagents
14.1.1 Boric acid (11): Add 100mL of sodium hydroxide, add 200ml of water..14,1.2 Magnetic acid (408/1.).
14.1.3 Take 2B sodium hydride, add platinum hydroxide (4g/I.), add water and dilute to 500mL. 14.1.4 Test paper: Weigh 20 ml of yellow powder, wash with cold water 4 times, store 100 ml each time. After removing the water-soluble substances, dry the residue. Add 1 ml of ethanol, wash, filter, take out a 1 mm filter paper strip, purify, take out, dry in air for 10 minutes, and put it on a glass plate. 14.2.1 Sample treatment Weigh 10 ml of solid sample, add sodium phosphate (4% sodium carbonate) to make it fully moist, dry it on a low fire, and then place it in a high temperature furnace for decomposition. Collect 10 ml of liquid sample. Dissolve it in carbonic acid (106/1) until it becomes magnetic, place it in a water bath for decomposition, and then place it in a commercial furnace for decomposition. 14. 2. 2 Qualitative test
14.2.2.1 Differential test paper method: Take all the ash, add a small amount of this and hydrochloric acid (1-1) until it is slightly acidic, stir while dripping, make the filter paper decompose, change the temperature and drain. Put the negative test paper into the filter, take out the test paper, and keep it warm. Dry it at 60℃~7℃ for a period of time. When sand is present, the test paper shows part or all color, and the part with color turns green immediately. 14.2.2.? Color should be: Mix the ash and add a few drops of ethanol, ignite directly, and when the acid becomes moist, the fire sample is green:
15 Hydrogen bridge acid
15.1 Reagents
15.1.1 Trinitride soft melt (11/1.). 15.1.2 Industrial nitric acid (.3) 1.7.
15.1.3 Ethylene (50%).
15.1.4 Pyrolysis of 102g/mol: limit 0g pyrolysis period (u, 5H0 hydrolyzed to 100258
15.2 Analysis steps
15.2.1 Sample grip
According to 3.1 of GB/TE009.28
32C3, after evaporating the acetaldehyde extract to dryness, set aside for use. 15. 2, 2 Qualitative test
GB/T 5009.29—2003
15.2.2.1 Ferric chloride method, add 1~2 drops of ferric chloride to the residual activity (:0R/1.3), and the color will be blue when salicylic acid is present. 15.2.2.2 Confirmation test: Dissolve in a small amount of hot water, cool, add 4~5 drops of sub-acid benzoate (1008/[.), 5 drops of acetic acid () and 1 drop of copper sulfate (150g/.>), drain, drain 0.5, and let stand for a while. The amount of water acid is blood red (mimicry acid is the color)4 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic half mean. 9.5 Others
Same as 5.6 of R/T5005.29-2003:
In: The third method is thin screen chromatography
10 Principle
After the sample is acidified, formic acid and sorbic acid are extracted with acetaldehyde. The sample extract is concentrated and spotted on a polyamide thin layer plate, opened, and after color development, the ratio of formic acid and sorbic acid on the thin layer plate is compared with the standard for qualitative analysis, and quantitative analysis can be performed. 236
11 Reagents
11.1 Isopropylamine sequence.
11.2 n-butyl alcohol
11.3 petroleum ether: boiling range 3c℃~60℃
1F.47: does not contain peroxide,
11.5 effective water.
11.6 anhydrous ethanol,
11.7 polyamide rubber powder: 200 liters.
13.8 Salt (1:), take 155mL with acid, add water to dilute to 200mL GD/T 5009.292003
11.9 Sodium chloride soluble alone (40%/1.): add 1% hydrochloric acid (:+1) to the sodium chloride filter (40R/1.) to acidify 11.10 Expand the following:
11.10.1 n-T alcohol + nitrogen water-anhydrous ethyl alcohol (71:2).11.10.2 isopropyl alcohol + hydrogen water-anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: accurately weigh 0.200% benzyl alcohol, dissolve it with a small amount of ethanol and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0 mg benzyl alcohol. 11.12 Standard solution of benzyl alcohol: accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0 mg benzyl alcohol. 11.13 Colorimetric test: 1% benzyl alcohol (in%) solution (0.4%/1 mL). Adjust to pH = 5 with sodium hydroxide solution (4 g/L). Preparation
12.1 Blow dryer!
12.2 Layer folding cylinder
12.3 Glass plate: 19am×18cm
12.4 Microinjection 10.100.
12.5 Sprayer.
13 Analysis Steps
13.1 Sample Extraction
Take 2.50 g of the first mixed sample and place it in a 25 mL dense tube: add 0.51 ml of hydrochloric acid (1 + 1) to acidify. Take 50 L of acetaldehyde twice, add 11 ml each time, and absorb the upper aldehyde into another 25 mL, fill the tube with dense filling, combine the acetaldehyde absorption liquid: wash the two drinks with 4 ml of chlorinated aldehyde (400 g/L), let it stand for 15 min, and use a dropper to filter the acetaldehyde layer through anhydrous flow to drain into a 25 mL container. Add acetaldehyde to the full scale, adjust, and absorb 15 ml of acetaldehyde into 1 μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1 centrifuge tubes m containing 1L of sample solution, set aside. 13.2 Determination
13.2.1 Preparation of sample powder plate: weigh 1.6g of acyl gelatin powder, add 0.4g of acetyl gelatin powder, add about 15ml of water, grind for 5min~5min, immediately put into the applicator to prepare two thin layer plates with a section of 10cm×1%cm and a thickness of c.3mm, dry at room temperature for 10min: dry for 1 hour: put in a dryer and keep. 13.2.2 Spotting: on the baseline 2m below the bottom of the thin layer plate, use a micro-radiograph to spot 1L and 2L of sample solution at the same time, and use 1L of the standard for acetic acid and formic acid.
13.2.3 Development and color matching: put the spotted plate into a developing solution pre-prepared with a developing agent (11.1.1 or 11.10.3). The filter paper around the developing area will remove the developing agent. The front edge is extended to 101 and then taken out of the turbidity. The color developer is sprayed, and the spots are yellow and the disk is blue. The amount of sorbic acid and benzoic acid contained in the material is compared with the standard point quantitatively (the specific values of sorbic acid and benzoic acid are 0.82 and 0.73 respectively). 2.37
CB/T5009.29--2003
13.3 Calculation
The total amount of sorbic acid or sorbitan in the test sample is measured by formula (3). X
mx is recorded in total!
The total amount of sorbitan in the test sample is in grams per kilogram [g/kA
The unit of the mass of the sorbitan in the test sample is bright grams (Mg) and the unit of the added sample is milliliters (m). The volume of the sample is measured in liters (mL)! Test air volume, unit is gram (g):
Timed strong collection of ethyl acetate to avoid the use of the report, unit is liter (ml.): The fresh sample is taken as described in the total supply, unit is liter (mI.). This method can also be used with the same method to determine the sample, to calculate the situation, use the commercial agent for qualitative test
14 Boric acid, ketoacyl
14.t Reagents
14.1.1 Boric acid (11): Add 100mL of sodium hydroxide, add 200ml of water..14,1.2 Magnetic acid (408/1.).
14.1.3 Take 2B sodium hydride, add platinum hydroxide (4g/I.), add water and dilute to 500mL. 14.1.4 Test paper: Weigh 20 ml of yellow powder, wash with cold water 4 times, store 100 ml each time. After removing the water-soluble substances, dry the residue. Add 1 ml of ethanol, wash, filter, take out a 1 mm filter paper strip, purify, take out, dry in air for 10 minutes, and put it on a glass plate. 14.2.1 Sample treatment Weigh 10 ml of solid sample, add sodium phosphate (4% sodium carbonate) to make it fully moist, dry it on a low fire, and then place it in a high temperature furnace for decomposition. Collect 10 ml of liquid sample. Dissolve it in carbonic acid (106/1) until it becomes magnetic, place it in a water bath for decomposition, and then place it in a commercial furnace for decomposition. 14. 2. 2 Qualitative test
14.2.2.1 Differential test paper method: Take all the ash, add a small amount of this and hydrochloric acid (1-1) until it is slightly acidic, stir while dripping, make the filter paper decompose, change the temperature and drain. Put the negative test paper into the filter, take out the test paper, and keep it warm. Dry it at 60℃~7℃ for a period of time. When sand is present, the test paper shows part or all color, and the part with color turns green immediately. 14.2.2.? Color should be: Mix the ash and add a few drops of ethanol, ignite directly, and when the acid becomes moist, the fire sample is green:
15 Hydrogen bridge acid
15.1 Reagents
15.1.1 Trinitride soft melt (11/1.). 15.1.2 Industrial nitric acid (.3) 1.7.
15.1.3 Ethylene (50%).
15.1.4 Pyrolysis of 102g/mol: limit 0g pyrolysis period (u, 5H0 hydrolyzed to 100258
15.2 Analysis steps
15.2.1 Sample grip
According to 3.1 of GB/TE009.28
32C3, after evaporating the acetaldehyde extract to dryness, set aside for use. 15. 2, 2 Qualitative test
GB/T 5009.29—2003
15.2.2.1 Ferric chloride method, add 1~2 drops of ferric chloride to the residual activity (:0R/1.3), and the color will be blue when salicylic acid is present. 15.2.2.2 Confirmation test: Dissolve in a small amount of hot water, cool, add 4~5 drops of sub-acid benzoate (1008/[.), 5 drops of acetic acid () and 1 drop of copper sulfate (150g/.>), drain, drain 0.5, and let stand for a while. The amount of water acid is blood red (mimicry acid is the color)9 Sodium chloride late solvent (40%/1.): Add a certain amount of hydrochloric acid (:+1) to the sodium chloride filter (40R/1.) to acidify 11.10. 11.10.1 n-Hydroxyethanol + nitrogen water-anhydrous ethyl alcohol (71:2). 11.10.2 Isopropyl alcohol + hydrogen water-anhydrous ethanol (7+1-2). 11.11 Standard solution of benzyl alcohol: accurately weigh 0.200% benzyl alcohol, dissolve it with a small amount of ethanol and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0 mg benzyl alcohol. 11.12 Standard solution of benzyl alcohol: accurately weigh 0.2000 benzaldehyde, dissolve it with a small amount of acetaldehyde and transfer it to a 100mL volumetric flask, and dilute to the mark. Each liter of this solution is equivalent to 2.0 mg benzyl alcohol. 11.13 Colorimetric test: 1% benzyl alcohol (in%) solution (0.4%/1 mL). Adjust to pH = 5 with sodium hydroxide solution (4 g/L). Preparation
12.1 Blow dryer!
12.2 Layer folding cylinder
12.3 Glass plate: 19am×18cm
12.4 Microinjection 10.100.
12.5 Sprayer.
13 Analysis Steps
13.1 Sample Extraction
Take 2.50 g of the first mixed sample and place it in a 25 mL dense tube: add 0.51 ml of hydrochloric acid (1 + 1) to acidify. Take 50 L of acetaldehyde twice, add 11 ml each time, and absorb the upper aldehyde into another 25 mL, fill the tube with dense filling, combine the acetaldehyde absorption liquid: wash the two drinks with 4 ml of chlorinated aldehyde (400 g/L), let it stand for 15 min, and use a dropper to filter the acetaldehyde layer through anhydrous flow to drain into a 25 mL container. Add acetaldehyde to the full scale, adjust, and absorb 15 ml of acetaldehyde into 1 μL centrifuge tubes twice: drain in a water bath at about 4°C, add 0 and 1 centrifuge tubes m containing 1L of sample solution, set aside. 13
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