International Oenological CODEX

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Cation exchange resins

COEI-1-RESECA Cation exchange resins

  1. Objective, origin and scope of application

Ion exchange is the reversible exchange of ions between a liquid and a solid, during the course of which the solid does not undergo any substantial changes.  When this technique is applied to wine, the solid is an insoluble, permeable synthetic resin capable of exchanging ions with the wine with which it is in contact.

These resins are used in the tartaric stabilization of wine.

  1. Composition

Cation exchange resins may be prepared in an appropriate physical form using one or more of the following formulas.

Sulfonated styrene-divinylbenzene copolymer:

Divinylbenzene-methacrylic acid copolymer

Resin inertia must be satisfactory.

The substances which can be used in the manufacture of these resins are indicated in Annexes 1 and 2.

The resin should not contain more than 1 mg of extractable organic substance per kg. These organic extracts are obtained with each of the following solvents: a) distilled water, b) alcohol, 15% by volume, c) 3% acetic acid solution (m/m).

The resin must have been washed and conditioned in accordance with the manufacturer's instructions.

Prepare different ion exchange columns for each solvent, using 50 ml of the resin that has previously been weighed.

While maintaining the maximum temperature that may be encountered during use, pass the three solvents used in the analysis (distilled water, 15% hydroalcohol ic solution and 3% acetic acid solution (m/m)) through the resins at a flow rate of 350-450 ml per hour.

The first liter of effluent from each solvent should not be considered for analytical purposes; only the following two liters of each solvent should be used to analyze the organic extracts.

Total extract: The two liter sample should be evaporated at 105 °C until a constant weight is obtained.

Ash: This dry residue derived drom evaporation of the 2 liters of effluent is then burned in an oven at 850 °C until a constant weight is obtained.

Organic extract: Total extract minus total ash gives the organic extract. If the organic extract is greater than 1 ml/l of solvent used, a "blank" should be made using the solvent and a correction should be made by subtracting the organic extract found in the "blank" from that obtained during the resin test. The solvents used are prepared as follows:

 

Control reagents: Distilled and/or de-ionized water.

Ethyl alcohol at 15% by volume obtained from absolute ethyl alcohol and distilled and/or de-ionized water.

3% acetic acid produced by mixing 3 parts (by mass) of acetic acid with 97 parts (by mass) of distilled and/or de-ionized water.

  1. Limits
  • The treatment must not alter the nature of the wine.
  • The treatmnt must not reduce the color intensity of the wine.
  • The treatment must not decrease the concentration of metallic cations in the wine below 300 mg/l.
  • The treatment must not lower the wine's pH below 3.0.  The decrease in pH should not exceed 0.3 pH units.
  • The resin must not leave substances in the wine or impart to it characteristics (as a result of the resin-based treatment) that do not ordinarily exist in wine.
  • The winemaker may use conditioning agents and/or regenerants composed of water and inorganic acids, bases or salts, provided that the conditioned or regenerated resin is washed in water until all conditioning agents and regenerants are removed before adding the wine.

Annex 1:List of substances used in the manufacture of adsorbant ion-exchange resins used to condition foodstuffs.

List 1Substances assessed by an international organization

Name

PM/REF

Case

Restrictions

Monomers and other

Starting substances

 

n-butyl acrylate

10780

00141-32-2

-

Ethyl acrylate

11470

00096-33-3

-

Acrylonitrile

12100

00107-13-1

SML = ND

(DL = 0.02 mg/kg)

SML = 15 mg/kg

Formaldehyde

17260

00050-00-0

  

Methyl methacrylate

21130

00080-62-6

-

Methanol

21550

00067-56-1

-

Styrene

24610

00100-42-5

-

Chemical Modifiers

Carbonic acid, salts

42500

-

-

Hydrochloric acid

72640

07664-38-2

-

Silicic acid, salts

85980

-

-

Sulfuric acid

91920

07664-93-9

-

Acetic anhydride

10150

00108-24-7

-

tert-butyl-4-hydroxyanisole (BHA)

40720

25013-16-5

SML=30 mg/kg

Diethylene triamine

15790

00111-40-0

SML= 5 mg/kg

Dimethylamine

49225

00124-40-3

SML=0.06 mg/kg

2-(dimethylamino)ethanol

49235

00108-01-0

SML=18 mg/kg

Formaldehyde

54880

00050-00-0

SML=15 mg/kg

Hexamethylenediamine

18460

00124-09-4

SML=2.4 mg/kg

Potassium hydroxide

81600

01310-58-3

-

Sodium hydroxide

86720

01310-73-2

-

Sodium nitrite

86920

07632-00-0

SML=0.6 mg/kg

Ethylene oxide

17020

00075-21-8

MQ=1 mg/kg in FP

2-propanol

81882

00067-63-0

-

Polymerization Additives

Akylsulfonic acids (C8-C22)

34230

-

SML=6 mg/kg

Linear, primary alkylsulfuric

34281

-

-

acids (C8-C22)  having an even number of carbon atoms

Formic acid

55040

00064-18-6

-

Carboxymethylcellulose

42640

09000-11-7

-

Stannic chloride(IV)

93420

07646-78-8

-

Methylene chloride

66620

00075-09-2

SML=0.05 mg/kg

1,4-dihydroxybenzene

48620

00123-31-9

SML=0.6 mg/kg

Gelatin

55440

09000-70-8

-

Ammonium hydroxide

35600

01336-21-6

-

Magnesium hydroxide

64640

01309-42-8

-

Hydroxyethylcellulose

60560

09004-62-0

-

Hydroxethylmethylcellulose

60880

09032-42-4

-

Methanol

65960

00067-56-1

-

Methylcarboxymethylcellulose

66200

37206-01-2

-

Methyl isobutyl ketone

66725

00108-10-1

SML=5 mg/kg

Toluene

93540

00108-88-3

SML=1.2 mg/kg

Annex 2: Substances that may be used provisionally to manufacture ion-exchange resins.

List 2

Substances not fully evaluated by an international organization

Name

PM/Ref

Case

Restrictions

Monomers and other starting

substances

Ethylene glycol dimethacrylate

20440

00097-90-5

-

Divinylbenzene

16690

01321-74-0

-

Diallyl ether of 1,1,1-tri- methylolpropane

25645

00682-09-7

-

2,3-epoxypropyl methacrylate

20590

00106-91-2

-

2-methyl-1,3-butadiene

21640

00078-79-5

-

1,7-octadiene

22585

03710-30-3

-

1,1,1-trimethylolpropane trimethacrylate

25840

03290-92-4

-

Chemical Modifiers

N,N-dimethyl-1,3-diamino- propane

49380

00109-55-7

-

Triethylamine

95270

00121-44-8

-

Triethylene tetramine

25520

00112-24-3

-

Polymerization Additives

Polyvinyl alcohols

81280

09002-89-5

-

4-tert-butylcatechol

40640

00098-29-3

-

Diisobutyl ketone

49050

00108-83-8

-

Sodium hypochlorite

62110

07681-52-9

-

Isobutanol

62270

00078-83-1

-

4-methoxyphenol

66030

00150-76-5

-

Methylene bis(sodium naphtha- lenesulfonate)

66600

26545-58-4

-

2-methyl-2-pentanol

66860

00108-11-2

-

Dibenzoylperoxide

46440

00094-36-0

  

Partially hydrolyzed vinyl polyacetate

81260

-

-

Substances not evaluated by an international organization

Name

PM/Ref

Case

Restrictions

Monomers and other starting substances

Dimethoxymethane

-

00109-87-5

-

Diethylene glycol divinyl ether

-

00764-99-8

  

Ethyl vinyl benzene

-

28106-30-1

-

1,2,4-trivinyl cyclohexane

-

02855-27-8

-

Chemical Modifiers

Chlorosulfonic acid

-

07790-94-5

-

Monochloroacetic acid

-

00079-11-8

-

Phosphoric acid

-

13598-36-2

-

Bromine

-

07726-95-6

-

2-chloroethanol

-

00107-07-3

-

Methyl chloride

-

00074-87-3

-

1,2-dichloroethane

-

00107-07-3

-

1,2-dichloropropane

-

00078-87-5

-

3-(dimethylamino)propane

-

03179-63-3

-

Name

PM/Ref

Case

Prescriptions

Monomers and other starting substances

Methylic chloromethyl ether

-

00107-30-2

-

Nitrobenzene

-

00098-95-3

-

Potassium nitrite

-

07758-09-0

-

Phthalimide

-

0085-41-6

-

Sulfur trioxide

-

07446-11-9

-

Trimethylamine

-

00075-50-3

-

Polymerization additives

Lignosulfonic acid

63940

08062-15-5

-

Peracetic acid

-

00079-21-0

-

Polyacrylic acid

76460

09003-01-4

-

Poly(styrenesulfonic) acid

-

09080-79-9

-

Acrylamide/acrylic acid copolymer

-

09003-06-9

-

Ethoxylated, propoxylated tert-alkylamines (C12-C14)

-

68603-58-7

-

Maleic anhydride-styrene copolymer, ammonium salt

-

26022-09-3

-

Attapulgite

-

12174-11-7

-

Azobisisobutyronitrile

-

00078-67-1

-

1,1-bis(tert-butylperoxy)-3,3,5- trimethylcyclohexane

-

06731-36-8

-

n-Dodecyl mercaptan

-

25103-58-6

-

Poly(ethylene/propylene)glycol monobutyl ester

-

09038-95-3

-

Polyethylene glycol octylphenyl ether

78560

09002-93-1

  

Poly(ethylene-propylene/glycol ether with 1,1,1-tromethylol-propane

-

52624-57-4

-

tert-hexadecyl mercaptan

-

25360-09-2

-

Cumyl hydroperoxide

-

00080-15-9

-

Isododecane

62405

31807-55-3

-

Isooctane

-

26635-64-3

-

Mono- and dialkyl (C10-C18) Sulfonamides

-

-

-

Silver nitrate

-

07761-88-8

-

n-Octane

-

00111-65-9

-

tert-Butyl peracetate

-

00107-71-1

-

tert-Butyl perbenzoate

-

00614-45-9

-

bis(4-tert-butylcyclohexyte) percarbonate tert

-

15520-11-3

-

Butyl per(2-ethyl-hexanoate)

-

03006-82-6

-

tert-Butyl peroctanoate

-

13467-82-8

-

Dilauroyl peroxide

-

00105-74-8

-

Poly(diallyldimethylammonium chloride

-

26062-79-3

-

Polyvinylpyrrolidone

81500

09003-39-8