CN110426488A - A kind of method of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food - Google Patents
A kind of method of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food Download PDFInfo
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- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention discloses a kind of methods of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food, comprising steps of 1) weighing 4.95~5.05g homogeneous sample or drawing 5.00~10.00mL fluid sample, are placed in distilling flask；2) 240~260mL water is added, 0.9~1.1mL of defoaming agent is added, loads onto condensing unit, under the liquid level for the iodine flask that the insertion of condenser pipe lower end has 22~28mL lead acetate absorbing liquid in advance, then 9~11mL hydrochloric acid solution is added in cucurbit, immediately lid plug, heating distillation；3) as 180~220mL of distillate, condenser pipe lower end is made to leave liquid level, 55~65S of redistillation；4) with the device part of a small amount of distilled water flushing insertion acetic acid lead solution；It is easy expansion blistering when solving rice flour class and the distillation of high protein substance, makes sample wall built-up, bubble seals in the problem of condenser pipe leads to the failure of an experiment.
Description
Technical field
The present invention relates to detection technique fields more particularly to a kind of GB 5009.34-2016 national food safety standard to examine
The method for surveying sulfur dioxide in food.
Background technique
The measurement of GB 5009.34-2016 national food safety standard sulfur dioxide in food.Sulfur dioxide detection distillation
In the process, rice flour class sample is easy foam expansion, flows into sample wall built-up even in condenser pipe, influences testing result.
Sulfur dioxide has Bleachability.Industrially commonly using sulfur dioxide comes bleached pulp, hair, silk, straw hat etc..Sulfur dioxide
Blanching effect be since its (sulfurous acid) can generate unstable colourless substance with certain coloring matters.This colourless substance holds
It easily decomposes and coloring matter is made to restore original color, therefore with the passing of time turned yellow again with the bleached plaited straw of sulfur dioxide.
The blanching effect of sulfur dioxide and certain sulfur-containing compounds also is illegally used to process food by some illegal manufacturers, so that food increases
It is white etc..Furthermore sulfur dioxide can also inhibit the growth of mould and bacterium, may be used as the preservative of food and dry fruit.But it is necessary
It is used in strict accordance with national relevant range and standard.Sulfur dioxide be allow both at home and abroad using a kind of food additives, usually
In the case of the substance with sulphite such as potassium metabisulfite, sodium pyrosulfite, sodium sulfite, sodium hydrogensulfite, Hydros
Form make an addition in food.The edible exceeded food of sulfur dioxide, has serious damage to liver, the kidney etc. of human body, and have carcinogenic
Effect.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to solve GB 5009.34-2016 " food safety country
Standard food sulphur dioxide measuring ", rice flour class and high protein substance are easy expansion blistering when distilling, make sample wall built-up, gas
Bubble seals in condenser pipe and leads to the failure of an experiment, can not in correct test sample content of sulfur dioxide problem GB 5009.34-2016
The method of national food safety standard detection sulfur dioxide in food.
In order to solve the above technical problems, the technical scheme is that
A kind of method of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food, comprising steps of
1) it weighs 4.95~5.05g homogeneous sample or draws 5.00~10.00mL fluid sample, be placed in distilling flask；
2) 240~260mL water is added, 0.9~1.1mL of defoaming agent is added, loads onto condensing unit, the insertion of condenser pipe lower end is pre-
Under the liquid level for first having the iodine flask of 22~28mL lead acetate absorbing liquid, 9~11mL hydrochloric acid solution is then added in cucurbit,
Lid plug immediately, heating distillation；
3) as 180~220mL of distillate, condenser pipe lower end is made to leave liquid level, 55~65S of redistillation；
4) with the device part of a small amount of distilled water flushing insertion acetic acid lead solution；
5) solution after absorbing is acidified with hydrochloric acid, and iodine standard solution titration consumes iodine standard solution amount according to titration, calculates
Content of sulfur dioxide in sample out.
The step 1) weighs 5g homogeneous sample as a preferred technical solution,.
The homogeneous sample is that distillation process stablizes vermicelli and distillation process not easy to foaming as a preferred technical solution,
The easily rice flour sample of expansion generation bubble.
250mL water is added in the step 2) as a preferred technical solution, defoaming agent 1mL is added, loads onto condensation dress
It sets, under the liquid level for the iodine flask that the insertion of condenser pipe lower end has 25mL lead acetate absorbing liquid in advance, is then added in cucurbit
10mL hydrochloric acid solution, lid plug, heating are distilled immediately.
The defoaming agent is the defoaming agent or not that organic silicone oil, ingredient are not involved in reaction as a preferred technical solution,
One of defoaming agent containing interfering substance, it is not miscible with water and most organic matters, to most of equal energy of bubble medium
Defoaming, it has preferable thermal stability, can use within the scope of 5 DEG C -150 DEG C broad temperature；Its chemical stability is preferable,
It is difficult that silicone oil can be used in acid, alkali, salting liquid with other substance reactions, it is that a kind of gathering for different polymerization degree chain structure is organic
Siloxanes.It is to add water to hydrolyze by dimethyldichlorosilane first minification polycyclic body is made, and low ring body is made through cracking, rectifying in ring body,
Then the mixtures of various different polymerization degrees just can be obtained in the telomerization of putting together of ring body, closure agent, catalyst, through being evaporated under reduced pressure
Silicone oil can be made by removing low-boiling-point substance.
Condenser pipe lower end is set to leave liquid level as distillate 200mL in the step 3) as a preferred technical solution,
Redistillation 60S.
By adopting the above-described technical solution, in a kind of GB 5009.34-2016 national food safety standard detection food
The method of sulfur dioxide, comprising steps of 1) weigh 4.95~5.05g homogeneous sample or draw 5.00~10.00mL fluid sample,
It is placed in distilling flask；2) 240~260mL water is added, 0.9~1.1mL of defoaming agent is added, loads onto condensing unit, under condenser pipe
Under the liquid level for the iodine flask that end insertion has 22~28mL lead acetate absorbing liquid in advance, 9~11mL is then added in cucurbit
Hydrochloric acid solution, lid plug, heating are distilled immediately；3) as 180~220mL of distillate, condenser pipe lower end is made to leave liquid level, redistillation
55~65S；4) with the device part of a small amount of distilled water flushing insertion acetic acid lead solution；5) solution after absorbing is acidified with hydrochloric acid,
Iodine standard solution titration consumes iodine standard solution amount according to titration, calculates content of sulfur dioxide in sample, solve
When GB5009.34-2016 " national food safety standard food sulphur dioxide measuring ", rice flour class and high protein substance distill
It is easy expansion blistering, makes sample wall built-up, bubble, which seals in condenser pipe, leads to the failure of an experiment, can not sulfur dioxide in correct test sample
The problem of content.
Specific embodiment
Embodiment 1
A kind of method of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food, feature exist
In, comprising steps of
1) it weighs 4.95g homogeneous sample or draws 5.00mL fluid sample, be placed in distilling flask；
2) 240mL water is added, defoaming agent 0.9mL is added, loads onto condensing unit, the insertion of condenser pipe lower end has 22mL in advance
Under the liquid level of the iodine flask of lead acetate absorbing liquid, 9mL hydrochloric acid solution is then added in cucurbit, immediately lid plug, heating distillation；
3) as distillate 180mL, condenser pipe lower end is made to leave liquid level, redistillation 55S；
4) with the device part of a small amount of distilled water flushing insertion acetic acid lead solution；
5) solution after absorbing is acidified with hydrochloric acid, and iodine standard solution titration consumes iodine standard solution amount according to titration, calculates
Content of sulfur dioxide in sample out.
The homogeneous sample is the rice that distillation process stablizes that vermicelli and distillation process not easy to foaming easily expand generation bubble
Powder sample.
The defoaming agent is organic silicone oil.
Embodiment 2
A kind of method of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food, feature exist
In, comprising steps of
1) it weighs 5.05g homogeneous sample or draws 10.00mL fluid sample, be placed in distilling flask；
2) 260mL water is added, defoaming agent 1.1mL is added, loads onto condensing unit, the insertion of condenser pipe lower end has 28mL in advance
Under the liquid level of the iodine flask of lead acetate absorbing liquid, 9~11mL hydrochloric acid solution is then added in cucurbit, immediately lid plug, heating
Distillation；
3) as distillate 220mL, condenser pipe lower end is made to leave liquid level, 55~65S of redistillation；
4) with the device part of a small amount of distilled water flushing insertion acetic acid lead solution；
5) solution after absorbing is acidified with hydrochloric acid, and iodine standard solution titration consumes iodine standard solution amount according to titration, calculates
Content of sulfur dioxide in sample out.
The homogeneous sample is the rice that distillation process stablizes that vermicelli and distillation process not easy to foaming easily expand generation bubble
Powder sample.
The defoaming agent is the defoaming agent without containing interfering substance.
Embodiment 3
A kind of method of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food, comprising steps of
1) it weighs 5g homogeneous sample or draws 5.00~10.00mL fluid sample, be placed in distilling flask；
2) 250mL water is added, defoaming agent 1mL is added, loads onto condensing unit, the insertion of condenser pipe lower end has 25mL second in advance
Under the liquid level of the iodine flask of lead plumbate absorbing liquid, 10mL hydrochloric acid solution is then added in cucurbit, immediately lid plug, heating distillation；
3) as distillate 200mL, condenser pipe lower end is made to leave liquid level, redistillation 60S；
4) with the device part of a small amount of distilled water flushing insertion acetic acid lead solution；
5) solution after absorbing is acidified with hydrochloric acid, and iodine standard solution titration consumes iodine standard solution amount according to titration, calculates
Content of sulfur dioxide in sample out.
The homogeneous sample is the rice that distillation process stablizes that vermicelli and distillation process not easy to foaming easily expand generation bubble
Powder sample.
The defoaming agent is the defoaming agent that ingredient is not involved in reaction.
Blank assay example:
Sample is acidified in closed container, is distilled, distillation is absorbed with acetic acid lead solution.Solution after absorption
It is acidified with hydrochloric acid, iodine standard solution titration consumes iodine standard solution amount according to titration, calculates content of sulfur dioxide in sample.
1.0ml defoaming agent testing result is added in 1 rice flour sample of table
Sample scalar quantity 0.10g/kg, recovery of standard addition 97.0%, Duplicate Samples relative average debiation < 10% comply with standard
It is required that.Conclusion: GB 5009.34-2016 " national food safety standard food sulphur dioxide measuring ", rice flour class and high protein
It is easy expansion blistering when substance is distilled, makes sample wall built-up, bubble, which seals in condenser pipe, leads to the failure of an experiment, can not correctly detect sample
Content of sulfur dioxide in product.By lot of experiments, the defoaming of 1.0mL dimeticone is added in distillation process in distilling flask
Agent keeps vapo(u)rizing temperature, and distillation process steadily carries out, and experiment success rate and efficiency is significantly improved, it was proved that defoaming agent
Addition will not influence sample itself content of sulfur dioxide, inspection result precision, accuracy meet national Specification.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
1. a kind of method of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food, which is characterized in that
Comprising steps of
1) it weighs 4.95~5.05g homogeneous sample or draws 5.00~10.00mL fluid sample, be placed in distilling flask；
2) 240~260mL water is added, 0.9~1.1mL of defoaming agent is added, loads onto condensing unit, the insertion of condenser pipe lower end is standby in advance
Under the liquid level for having the iodine flask of 22~28mL lead acetate absorbing liquid, 9~11mL hydrochloric acid solution is then added in cucurbit, immediately
Gai Sai, heating distillation；
3) as 180~220mL of distillate, condenser pipe lower end is made to leave liquid level, 55~65S of redistillation；
4) with the device part of a small amount of distilled water flushing insertion acetic acid lead solution；
5) solution after absorbing is acidified with hydrochloric acid, and iodine standard solution titration consumes iodine standard solution amount according to titration, calculates examination
Content of sulfur dioxide in sample.
2. the side of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food as described in claim 1
Method, it is characterised in that: the step 1) weighs 5g homogeneous sample.
3. the side of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food as claimed in claim 2
Method, it is characterised in that: the homogeneous sample is that distillation process stable vermicelli and distillation process not easy to foaming easily expand generation gas
The rice flour sample of bubble.
4. the side of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food as described in claim 1
Method, it is characterised in that: 250mL water is added in the step 2), defoaming agent 1mL is added, loads onto condensing unit, condenser pipe lower end is inserted
Under the liquid level for entering the iodine flask for having 25mL lead acetate absorbing liquid in advance, 10mL hydrochloric acid solution is then added in cucurbit, stands
That is lid plug, heating distillation.
5. the side of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food as claimed in claim 4
Method, it is characterised in that: the defoaming agent is organic silicone oil, ingredient is not involved in the defoaming agent of reaction or without containing interfering substance
One of defoaming agent.
6. the side of GB 5009.34-2016 national food safety standard detection sulfur dioxide in food as described in claim 1
Method, it is characterised in that: in the step 3) as distillate 200mL, condenser pipe lower end is made to leave liquid level, redistillation 60S.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257502A (en) * | 2020-03-05 | 2020-06-09 | 江苏权正检验检测有限公司 | Method for measuring sulfur dioxide in dried mushrooms |
| CN113391026A (en) * | 2021-06-11 | 2021-09-14 | 北京华澳维科技有限公司 | Rapid distillation method and detection method for sulfur dioxide |
-
2019
- 2019-07-30 CN CN201910694628.9A patent/CN110426488A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257502A (en) * | 2020-03-05 | 2020-06-09 | 江苏权正检验检测有限公司 | Method for measuring sulfur dioxide in dried mushrooms |
| CN113391026A (en) * | 2021-06-11 | 2021-09-14 | 北京华澳维科技有限公司 | Rapid distillation method and detection method for sulfur dioxide |
| CN113391026B (en) * | 2021-06-11 | 2023-08-15 | 北京华澳维科技有限公司 | Sulfur dioxide rapid distillation method and detection method |
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