This standard specifies the determination method for the residue of germination inhibitor in tobacco and tobacco products. This standard is applicable to the determination of the residue of germination inhibitor in tobacco and tobacco products. GB/T 19611-2004 Determination of the residue of germination inhibitor in tobacco and tobacco products UV spectrophotometry GB/T19611-2004 Standard download decompression password: www.bzxz.net

Irs 65.160
National Standard of the People's Republic of China
GB/T19611—2004
Tobacco and tobacco products
Deter'mination of malelc hydrazide residues-Uy spectrophotometer method
(IS0 4876:1980.M0D)
2004-12-14 Issued
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China Standardization Administration of China
2005-03-01 Implementation
This standard adopts the international standard IS04876:1950% smoke vehicle modified smoke or product GB/r19611-2004
For convenience, compared with 804719%, this standard has made the following changes to the standard name, \common name of \common name should be \common name ... Except for IS04876: 0% before:
Except for TS04876, 8) reference materials:
A training plan specification document is not a use document, and the use standard adopts the international standard that has been transformed into a national cup standard or industry standard. This standard is recorded in the A layer of the specification - Appendix T is the goods except for the record. The national tobacco standardization technical committee (744) is in charge of this standard. The unit of this standard is: the national tobacco standard inspection center. The second standard soil Liang Qi myself, Zhang Cheng, Lu Ci Ling, Zhu Shuizi Xu Kuan, Hao Wei, Liu Huimin 1 Scope
Tobacco and tobacco Determination of the amount of inhibitory amine residues in hay products by ultraviolet spectrophotometry
This standard is based on the determination method of inhibitory amine residues in hay products. This standard is applicable to the determination of the amount of inhibitory amine residues in hay products. 2 Normative referenced documents
GR/T19611—2004
The following clauses are cited as the clauses of this standard and are the reference documents of this standard. All subsequent revisions (excluding other omissions) or revised editions shall not apply to this standard. However, the parties who have reached an agreement based on this standard may use the new edition of this document. The latest version of the standard is applicable to the following standards: (3/T19616-2301-15) 4874.2220.M0) C:3: Tobacco and tobacco products test machine - single label full bottle method (YL[31-1U96, 1S078811S92, 156) 1042 Laboratory apparatus - single label full bottle 1S() 4703 Laboratory overview (multiple standard > through the instrument letter. Classification and nomenclature 3 Physical || tt || The sample is devolatile at the midpoint of the sodium hydroxide solution. Added to the granules, the inhibitor is reduced to butane by new hydrogen, which is then hydrolyzed and released into a yellow compound with 1-methylaminoformyl. If necessary, the sample can be optically disinfected with acid and purified with an active magnetic agent. 4 Reagents and Materials
Use pure reagents, water or equivalent: 4.11 Hydrogen hydride solution, each liter of 1.5mol/L sulfuric acid solution can contain 20g 2.1.1 Preparation of pure reagents: Weigh 23.00-aminobenzene and dissolve it in 150ml of water, add 5g of active ingredient, filter it with a cloth, add 2% water to the solution, precipitate it with a filter, and press 5ml. Rinse the product with cold water, transfer it to a desiccator, and store it in a dark medium for later use
4.1.2 Preparation: Weigh the product mentioned in 7.01 and add 100ml, 1mol/L slightly acid solution (4%, if necessary, use burning The result is that the speed of the reaction is too fast and the reaction is not too fast. The reaction is stored in a refrigerator away from light. It should not be prepared. 4.2 The standard of the seed bud is not, g/L. Take 0mg pH to 2: mg group in 103L0.1mnl/aqueous sodium hydroxide solution: 1. Sieve water to 10CcmL
4.3 Cold particles, 500Am. Standard density is not more than 1.70/n, the purity of the duo is very safe, and the inspection is carried out. The color of the sulphur and nitrogen in the standard method can be compared with the color of the three-color sulphur sulphur sulphur produced by reduction and group addition
4.4 The gaseous body is filtered, 135t:01/., 4.5 Hydrogen hydride chain, .1mol/L
4.6 The density of microparticles is 0.m/
GB/T 19611—2004
4.7 Iron oxide tetrahydrate (FeCl2,·41L)): It does not react with trichloroethylene to form aldehydes. 4.3 Anti-foaming agent (liquid foaming agent or bamboo foaming agent). 4.9 Explosion-proof oxygen porcelain, right), 4.10 With the waste plan, Asia and then high full point shrimp straight sesame oil), 4.11 Plan, remove the beauty, and only with the key sample (7, 4 similar characteristics. 5-position instrument, commonly used experimental level instrument and the following items, 5.1 volumetric bottle, 25rL, 10)m..122)ml according to I5)1042A requirements, 5.2 to, 100.1. 5.3 filter damage 250L 5.4 cloth ratio sintering fracture degree level P1 00, according to the requirements of 15) 4793 5.5 water vapor steam filling installation see Figure 1
heat preservation type decay
introduction quality technology type
clean environment into
introduction of water application
Figure 1 inhibitory bud determination loading diagram
water vapor steam rumor equipment, including:
steam generator,
reaction / hot distillation bottle:
cold general once
adjustment furnace,
reaction / hot is 5uml. flat thick villa flask, with a thermometer in the hole to pick a thermometer. The steam generator is used to react / use the bottle through a standard connection, the third one is used not to introduce room water, so that when the area should / algae tank is replaced, the hot steam generation end can maintain a stable speed. 5.6 Spectrophotometer. It can measure the absorbance at 425nm, 455nm and 485nm, and is equipped with a 10mm colorimeter. 5. Sample preparation
Press /Tle to take samples:
7. Operation steps
7.1 Sample preparation
Press Y to prepare the sample for determination of the moisture content of the sample. 7.2 Test material
Take 1 sample and transfer it to the sample, and the sample should be as fine as possible. 7.3 Determination
Before digestion, use glandular digestion (see Appendix A). GB/T:19611—2004
7.3.1 Reduce digestion
Put the selected product in a bottle, add 0m. sodium hydroxide solution (4.4), a little precautionary agent (.%>) and a few tablets of precautionary agent (4.), insert the thermometer into the empty high boiling point correction (2.10) medicine. Heat carefully, stirring the sample from time to time, keep heating enough to reduce the stirring in the bottle, until the temperature reaches 165. It takes about 10min~.15min. Then After cooling for 3min, add 10L of acid solution (4.6) to the steam generator. Use the tube (5.2) as the receiver, add 5L of chlorinated arsenic (4.7) and 1L of zinc granules (1.3) to the conical flask and connect the conical flask with the steam generator. Let the steam enter the flask and heat the sample at 200℃ for 10min. During the heat increase, the condenser should be fully condensed. The rapid evaporation flask always maintains 200℃ to ensure that 10mL of effluent is received in 20min. Rinse the condensation micro-tube with water and combine it with the effluent. Cool and distill. Use the Brinell glass tube (5.4) to rinse the effluent with 250mL of water and then rinse the effluent with 5mL of water. In a small amount of burning beaker, boil the sample on an electric furnace until the final volume is 6 ml (not less than 6 ml). The liquid can be rotated to make sure the liquid is not changed. Before the next change, the liquid can be oxidized overnight. See Appendix. 7.3.3 Reaction with 4-dimethylaminobenzyl alcohol. Cool the obtained solution in 7.3.2 and transfer it to 251 ml (F, 1). The yield is 10. Add 2 mL of 4-dimethylaminobenzyl alcohol (4.1) and adjust the concentration with water. Put the volume into the bottle tightly, stir it and measure it with a spectrophotometer in the dark. Add 10 mL of sulfuric acid (+6) and 2 mL of 1 ...4-Hydroxyformaldehyde is placed in a 2m3/s container with water. The standard deviation is: take the northern liquid as the reference liquid. The same spectrophotometer has the same absorbance at 425nm, 2nm and 485nm. The calibration formula A is used to calculate the calibration deviation of the liquid. Where A/A is used for the sample at 425nm, 43nm and 45nm respectively. If the absorbance at 155nm exceeds the range (K), the reference ratio should be used as soon as possible. The following will be detailed The sample should be measured in parallel twice. 7.4 Standard curve
Add 0.1ml.2rmI of standard 1% ...
Where:
Standard is the mass of the sample collected by the cable, in grams (cell);
Sample moisture content.% (quantity).
Calibration is performed during the analysis: 7..1: www.bzxz.net
Use the average value of the two half-step results as the step result, and the reproducibility should meet the requirements of 3.2. 8.2 Repeat the
currency to an operator for two consecutive operations at the same time. The difference between the test results shall not exceed 5% when the average value is 10/g, and may exceed 1.9% when the average value is 10/g. The test report shall include the method used and the results obtained. The report shall also include any operating conditions not specified or selected by the party (such as special types described in the appendix) and other conditions that may affect the results. The sample reported shall be for production data only. 4.1 General tt||Yang Ling A
(Normative Appendix)
Optional Supplementary Materials
CB/I19G1I—2004
4.1.1 Avoid the occurrence of large amounts of foam when the protein is digested and the amount of foam produced. 2 The acid pre-digestion method can distinguish the protein and produce less liquid foam.
A, 1.2 The content of some special ingredients is sufficient, and the color reaction is natural, and the formula is 1- Dimethylformaldehyde reacts with acetaldehyde to produce a red color. Use carbon dioxide as described in A.3. 4.1.3 Unless the analyst believes that the sample to be tested requires it: This operation is generally not required. A.2 Acid predigestion
A2.1 Reagents
4.2.1.1 Hot solution. mol/]. Dilute 273nml of acid with water to 10mL. A2.1. E sodium hydroxide solution, 71/mol/.
A.2.7 Operation steps
Transfer the sample to the reaction mixture. Add talc (A2.: 1) and a certain amount of sodium hydroxide solution: Heat the mass to filter slowly until the liquid volume is reduced to 20~25mL: Wash the bottle with 35L water: Repeat the process until the liquid volume in the bottle is reduced to -.25 a. Stop and cool.
The partially digested sample can be placed in the society, and the whole environment is completed. There is a liquid (eight, 2, 2, and the loss is added) and then the digestion is carried out according to 7.1. 1.3 Activated carbon purification
1.3. 1 Reagents
A. 3. 1. 1 Activated carbon
A.3.2 Operation steps
Mix 75.2 of the obtained clinical product with 2g of activated carbon, filter it by 1mi and concentrate it in a micro-box according to 7.3.3. GR/T19611—2004
Record B
(Informative Appendix)
Precautions for bacterial adjustment operation
B.1 After the safety barrier is changed to the dead crown, B2 is added to the node, collect the hot zone bottom adjustment bottle at the time of your teaching and anti-diffusion environment, take the temperature of the meter , use a small unplugged gas meter socket to clean the gas carrier pipe, and collect the remaining residue in the reaction solution into the wire mesh in the water. Rinse the solution twice with water, and then use 1 liter (partial volume) of liquid to remove large solid alkali and particles. Fill the solution with concentrated hydrochloric acid until it is ready for use again, and rinse the solution once with water. This is done to remove any zinc particles that may be left in the solution, as they will cause premature decomposition in the digestion stage during the next measurement.1. After the safety barrier is changed to the B2 cable node, adjust the temperature of the bottle to the bottom of the hot zone and prevent the expansion of the environment, take the temperature meter, use a small unplugged seat temperature meter socket, wash the cable on the steam-carrying tube, and collect the remaining residue in the wire mesh in the water. Rinse the network twice with water, and then use 1 (amount of liquid) to remove the solid alkali and particles. Fill the flask with concentrated hydrochloric acid until it is fully filled, and rinse it with water before using it again. This column is made to remove the zinc particles that may be left in the flask, which will cause premature decomposition in the digestion stage during the next measurement.1. After the safety barrier is changed to the B2 cable node, adjust the temperature of the bottle to the bottom of the hot zone and prevent the expansion of the environment, take the temperature meter, use a small unplugged seat temperature meter socket, wash the cable on the steam-carrying tube, and collect the remaining residue in the wire mesh in the water. Rinse the network twice with water, and then use 1 (amount of liquid) to remove the solid alkali and particles. Fill the flask with concentrated hydrochloric acid until it is fully filled, and rinse it with water before using it again. This column is made to remove the zinc particles that may be left in the flask, which will cause premature decomposition in the digestion stage during the next measurement.
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