CN101430288B - Sulphur dioxide measuring equipment used for food - Google Patents

Sulphur dioxide measuring equipment used for food Download PDF

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Publication number
CN101430288B
CN101430288B CN2008102443780A CN200810244378A CN101430288B CN 101430288 B CN101430288 B CN 101430288B CN 2008102443780 A CN2008102443780 A CN 2008102443780A CN 200810244378 A CN200810244378 A CN 200810244378A CN 101430288 B CN101430288 B CN 101430288B
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China
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pipe
communicated
condenser
measuring equipment
sulphur dioxide
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Expired - Fee Related
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CN2008102443780A
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CN101430288A (en
Inventor
郑屏
盛旋
胡艳云
余晓峰
陈昌骏
张蕾
孙昊
姚剑
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ANHUI ENTRY-EXIT INSPECTION AND QUARANTINE BUREAU PEOPLE'S REPUBLIC OF CHINA
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ANHUI ENTRY-EXIT INSPECTION AND QUARANTINE BUREAU PEOPLE'S REPUBLIC OF CHINA
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Abstract

The invention relates to a device used for mensurating sulfur dioxide in food. The device solves the problems that the sulfur dioxide in a product with the high content of organic acid and a sample containing organic sulfur component can not be mensurated, and organic substance interference exists during the mensuration. The device comprises a liquid storage funnel. A liquid outlet at the bottom of the liquid storage funnel is communicated with a three-way pipe, one lateral pipe opening of which is a nitrogen input port, and a lower end of a conductor which is communicated with the other pipe opening is arranged in a distillation flask. The top of the distillation flask is communicated with a condenser tube inlet of a condenser, and a condenser tube outlet is communicated with a vent pipe. A cooling water cover covers over the outside of the condenser tube, and the cooling water cover is provided with a water outlet at the upper part and is provided with a water inlet at the lower part. The vent pipe is connected with four branch pipes in series by four three-way pipes, and each branch pipe extends into an absorption bottle respectively. The device can be used for mensurating the product with the high content of the organic acid and the sample containing the organic sulfur, and the device can eliminate the interference caused by the organic substance when mensurating the sulfur dioxide in food. The device is safe and convenient for operating, and reagents in use are all nontoxic and harmless and meet the requirement of environmental protection.

Description

The sulphur dioxide measuring equipment that is used for food
Technical field
The present invention relates to be used for the pick-up unit that sulfur dioxide in food detects.
Background technology
The main method that is applied to sulfur dioxide in food mensuration at present is hydrochloric para-rosaniline method, distillation iodimetric titration, formaldehyde iodimetric titration and distillation alkali titration.The shortcoming of these methods is as follows:
1. hydrochloric para-rosaniline method.
Cardinal principle is to measure by spectrophotometer in conjunction with colour developing by hydrochloric acid Pararosaniline and sulphuric dioxide again.There is following shortcoming in this method:
1), color development system shakiness, poor reproducibility, cause testing result to occur often than mistake.
2), detection time is long time-consuming, a whole set of test operation duration is more than 5.5 hours, is not suitable for field quick detection.
3), some problems that also exist in the reagent preparation:
4), use poisonous solution in the test, operator and environment are worked the mischief.
2. distillation iodimetric titration
In closed container sample is carried out acidifying and adds thermal distillation, to discharge sulphuric dioxide wherein, releaser absorbs with lead acetate solution.Absorb the back and use the concentrated acid acidifying,, calculate the content of the sulphuric dioxide in the sample according to the iodine standard solution amount that is consumed again with the iodine standard solution titration.Method required reagent easy and simple to handle and instrument are less, but also have some problems:
1), for some sample such as dried thin mushroom sample, in still-process, the lead acetate absorption liquid becomes black, has covered blueness after adding starch indicator, causes titration end-point to be difficult to judge, so its determination data precision is relatively poor.
2), the distillation iodimetric titration sample preparation too simple, this makes that this method recovery is not high.
3. formaldehyde iodimetric titration
Tested composition sulphuric dioxide (comprising combined state and free state) in the sample loses binding ability in alkali lye, be fixed to sulphite; Under the effect of sulfuric acid, make it dissociate out again, and carry out titration with iodine mark liquid; When reaching titration end-point, excessive iodine and starch indicator effect generate blue iodine-starch compound.Calculate the amount of Total sulfur dioxide by the titer of iodine mark liquid.The main weak point of some of formaldehyde iodimetric titration is:
1), be subjected to the influence of acidity,
2), be subjected to the influence of formaldehyde consumption,
3), the endpoint difficulty,
4), the sample preparation mode has problems.
4. distillation-alkali titration
Acidifying heating and decomposition testing sample discharges SO in nitrogen stream 2, bubbling is by absorbing and oxidation the NaOH titration of concentration known of the sulfuric acid of generation in neutral rare hydrogen peroxide.
Part jointly comes with some shortcomings:
1), organic acid disturbs these two kinds of method measurement results influences very greatly, so the gravimetric method conclusive evidence method of having replenished regulations, this has greatly prolonged sense cycle, influences sample analysis speed.
2), these two kinds of methods are all inapplicable for the spice of the sample that contains the organic sulfur component such as garlic goods, green onion ginger and other kinds.
Also there be not at present a kind of detection method and determinator that is applicable to all food products, the sample that does not particularly have to measure the high product of organic acid content and contain the organic sulfur component, the sample of the interference that organism brings when not having to eliminate the mensuration sulfur dioxide in food.
Summary of the invention
In order to solve the high product of organic acid content and to contain the sulphur dioxide measuring problem of the sample of organic sulfur component, and organism brings the problem of interference when measuring, and the invention provides a kind of novel sulphur dioxide measuring equipment that is used for food.
Concrete structural design scheme is as follows:
The sulphur dioxide measuring equipment that is used for food comprises a storage liquid funnel, and its top bottleneck is provided with bottle stopper, and its bottom liquid outlet is being communicated with three-way pipe, and the liquid outlet place of storage liquid funnel is provided with the flow rate regulation piston;
One side pipe mouth of described three-way pipe is the nitrogen input port, opposite side mouth of pipe connecting duct, and the lower end of conduit is located in the distilling flask;
Described distilling flask top is being communicated with the condenser pipe inlet of condenser, the condenser pipe of condenser exports a side and is being communicated with gas outlet, opposite side is being communicated with the bottle mouth position of storing the liquid funnel, the condenser pipe outer cup of described condenser is provided with the chilled water cover, chilled water cover top is provided with water delivering orifice, and the bottom is provided with water inlet;
By four three-way pipes, four arms of connecting, each arm stretches into respectively in the absorption bottle on the described gas outlet, and the gas outlet another port is an exhausr port.
Described storage liquid funnel is the cylinder ampuliform, and diameter is 45 millimeters, highly is 120 millimeters.
The capacity of described distilling flask is 500 milliliters, and its bottleneck is not less than 150 millimeters apart from the height of bottom surface.
The described conduit lower end mouth of pipe that stretches in the distilling flask is not less than 10 millimeters apart from the distance of distilling flask bottom surface.
Described condenser pipe is a spiral pipe, and the spiral pipe total length is not less than 250 millimeters, and the spiral number of turns is not less than 10 circles.
Described absorption bottle is the big waist drum bottle in middle part small in ends, and its middle part diameter is 50 millimeters, and the middle part highly is 75 millimeters, and lower diameter is 18 millimeters, and lower height is 20 millimeters.
The following pipe end of described arm is the spray head.
Mensuration usable range of the present invention expands to all food products, comprises high product of organic acid content and the sample that contains the organic sulfur component, can eliminate the interference that organism brings when measuring sulfur dioxide in food.Handling safety, convenience, agents useful for same are all nontoxic, compliance with environmental protection requirements.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described by embodiment.
Embodiment:
Referring to Fig. 1, the sulphur dioxide measuring equipment that is used for food comprises a cylinder ampuliform storage liquid funnel 1, and diameter is 45 millimeters, highly is 120 millimeters.Its top bottleneck is provided with bottle stopper, and its bottom liquid outlet is being communicated with three-way pipe, and the liquid outlet place of storage liquid funnel is provided with the flow rate regulation piston, with the controlling liquid flow velocity;
One side pipe mouth of three-way pipe is nitrogen input port 2, opposite side mouth of pipe connecting duct, and the lower end of conduit is stretched in the distilling flask 3; The capacity of distilling flask is 500 milliliters, and its bottleneck is not less than 150 millimeters apart from the height of bottom surface, and the conduit lower end mouth of pipe that stretches in the distilling flask is not less than 10 millimeters apart from the distance of distilling flask bottom surface.
Distilling flask 3 tops are being communicated with the condenser pipe inlet of condenser 4, and the condenser pipe of condenser exports a side and is being communicated with glass exhaust tube, and opposite side is being communicated with the bottle mouth position of storing the liquid funnel by glass tube, with intensifier intensity; Condenser pipe is a spiral pipe, and the spiral pipe total length is not less than 250 millimeters, and the spiral number of turns is not less than 10 circles; The condenser pipe outer cup of condenser is provided with the chilled water cover, and chilled water cover top is provided with water delivering orifice, and the bottom is provided with water inlet, connects tap water during use;
On the gas outlet by four three-way pipes, four arms of connecting, i.e. first arm, second arm, the 3rd arm and the 4th arm, and stretching into respectively in first absorption bottle, second absorption bottle, the 3rd absorption bottle and the 4th absorption bottle, the following pipe end of four arms is the spray head.First absorption bottle and second absorption bottle are that absolute ethyl alcohol purifies absorption bottle, the 3rd absorption bottle and the 4th absorption bottle are the hydrogen peroxide absorption bottle, absorption bottle is the big waist drum bottle in middle part small in ends, its middle part diameter is 50 millimeters, the middle part highly is 75 millimeters, lower diameter is 18 millimeters, and lower height is 20 millimeters; The gas outlet another port is an exhausr port.
Using method: take by weighing the 20g sample, place distilling flask 3, in the 3rd absorption bottle 7 and the 4th absorption bottle parts 8, add 3mL concentration respectively and be 6% superoxol and the blue indicator of 0.1mL bromophenol, with the NaOH titration superoxol of concentration 0.01mol/L to neutral.Respectively add the 10mL absolute ethyl alcohol at first absorption bottle 5 and second absorption bottle 6, in storage liquid funnel 1, add 100mL water and 5mL hydrochloric acid solution, logical nitrogen is with the air emptying of distilling flask 3 and whole device, open the flow rate regulation piston of storage liquid funnel 1, drips of solution in the storage liquid funnel 1 is added in the distilling flask 3, if needed, temporary close nitrogen stream.
Slow heating distilling flask 3 to solution wherein seethes with excitement, heating 45min is continued in the boiling back, in whole process, keep the nitrogen flow rate degree, after heating finishes, merging the solution in the 3rd absorption bottle 7 and the 4th absorption bottle parts 8, is the sodium hydroxide solution titration of 0.01mol/L or 0.1mol/L with concentration, obtains the amount of substance of sulphuric dioxide in the sample by the volume that consumes sodium hydroxide solution.
Exhaust is discharged from the exhausr port of gas outlet.

Claims (7)

1. be used for the sulphur dioxide measuring equipment of food, it is characterized in that: comprise a storage liquid funnel, its top bottleneck is provided with bottle stopper, and its bottom liquid outlet is being communicated with three-way pipe, and the liquid outlet place of storage liquid funnel is provided with the flow rate regulation piston;
One side pipe mouth of described three-way pipe is the nitrogen input port, opposite side mouth of pipe connecting duct, and the lower end of conduit is located in the distilling flask;
Described distilling flask top is being communicated with the condenser pipe inlet of condenser, the condenser pipe of condenser exports a side and is being communicated with gas outlet, opposite side is being communicated with the bottle mouth position of storing the liquid funnel, the condenser pipe outer cup of described condenser is provided with the chilled water cover, chilled water cover top is provided with water delivering orifice, and the bottom is provided with water inlet;
By four three-way pipes, four arms of connecting, each arm stretches into respectively in the absorption bottle on the described gas outlet, and the gas outlet another port is an exhausr port.
2. the sulphur dioxide measuring equipment that is used for food according to claim 1 is characterized in that: described storage liquid funnel is the cylinder ampuliform, and diameter is 45 millimeters, highly is 120 millimeters.
3. the sulphur dioxide measuring equipment that is used for food according to claim 1 is characterized in that: the capacity of described distilling flask is 500 milliliters, and its bottleneck is not less than 150 millimeters apart from the height of bottom surface.
4. the sulphur dioxide measuring equipment that is used for food according to claim 1 is characterized in that: the described conduit lower end mouth of pipe that stretches in the distilling flask is not less than 10 millimeters apart from the distance of distilling flask bottom surface.
5. the sulphur dioxide measuring equipment that is used for food according to claim 1 is characterized in that: described condenser pipe is a spiral pipe, and the spiral pipe total length is not less than 250 millimeters, and the spiral number of turns is not less than 10 circles.
6. the sulphur dioxide measuring equipment that is used for food according to claim 1 is characterized in that: described absorption bottle is the big waist drum bottle in middle part small in ends.
7. the sulphur dioxide measuring equipment that is used for food according to claim 1 is characterized in that: the following pipe end of described arm is the spray head.
CN2008102443780A 2008-11-28 2008-11-28 Sulphur dioxide measuring equipment used for food Expired - Fee Related CN101430288B (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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CN101430288A CN101430288A (en) 2009-05-13
CN101430288B true CN101430288B (en) 2010-09-08

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Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103372325B (en) * 2013-08-08 2015-06-03 中华人民共和国梧州出入境检验检疫局 Water distillation apparatus
CN104198485A (en) * 2014-08-16 2014-12-10 中山鼎晟生物科技有限公司 Rapid detection method of sulfur dioxide in Lycium barbarum fruits
CN104297243A (en) * 2014-10-18 2015-01-21 中山鼎晟生物科技有限公司 Method applied to rapid detection of sulfur dioxide in wine products
CN104677712B (en) * 2015-03-30 2017-06-16 天津出入境检验检疫局动植物与食品检测中心 Liposoluble vitamin sample determination pretreating device and method in Milk Powder Formula For Infants
CN106872236B (en) * 2017-04-07 2024-01-26 北京普立泰科仪器有限公司 Sulfur dioxide automatic extraction device
CN109187846B (en) * 2018-08-31 2024-01-30 江苏省送变电有限公司 Sealed sample injection device for detecting acidity of sulfur hexafluoride gas
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

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