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SO2 is used as preservative in the food industry, especially in beverages such as fruit juices and wine as well

as dried fruit and vegetables. The maximum amount of SO2 is limited by law due to severe health risks. The
EC guidelines requires the labelling of SO2 at concentrations more than 10 mg/kg or 10 mg/L.

Total sulphur dioxide is liberated by acidic steam distillation and is fixed and oxidized by hydrogen peroxide. The
sulphuric acid formed is determined by titration with standardized sodium hydroxide.

Sample types:
 Liquid samples: wine, soft drinks, fruit juice, beer, must
 Solid and semi solid samples: dried apricot, celery, jams, syrups, sausages, burgers
Detection limit: 5 mg/L

Wear gloves (PPE’s) and eye protection while handling phosphoric acid, hydrogen peroxide and sodium hydroxide.
Follow safety instruction of instrument user manuals and Material Safety Data Sheets.

4.1 Foss Kjeltec Distillation systems:


KjeltecTM 2100 Distillation unit
KjeltecTM 2200 Auto distillation unit
KjeltecTM 8100 Distillation unit
KjeltecTM 8200 Auto distillation unit
NOTE: If sulphite determinations are commonly performed the silicone tubing from the splash head to the
condenser should be replaced with Viton tubing (article number 1582-0001)
4.2 750 ml distillation tubes
4.3 25 ml burette (or equivalent)
4.4 250 ml Erlenmeyer flask
4.5 Analytical balance

5.1 60 % phosphoric acid


Weigh 1042 g of deionised water into 4 L plastic beaker
Add 2.5 L 85 % phosphoric acid
NOTE: For safety and environmental reason phosphoric acid can be replaced by 50 % citric acid
5.2 Titrant
0.01 N or 0.05 N Sodium Hydroxide (standardized)
NOTE: The normality of the titrant is required to 4 decimal places.
5.3 Receiver solution:
Hydrogen peroxide solution (add 200 ml 35 % H2O2 to 1L distilled H2O)
Add 10 ml indicator solution (100 mg methyl red, 50 mg methylene blue in 100 ml ethanol)
NOTE: The receiver solution should be freshly prepared.

Adjust sample to room temperature. For liquid samples dissolved CO2 is removed by shaking sample vigorously, or
by using ultrasonic bath for degassing. For solid samples cut sample in small pieces. Avoid unnecessary exposure to
air.

For details see user manual

Model Dilution Phosphoric Delay SAfE Distil Distillation % Steam


acid end
condition
2100 50 ml 30 ml 12 s 5s 4 min time 100
2200 50 ml 30 ml 12 s 5s 4 min time 100
8100 50 ml 30 ml 12 s 5s 5 min time 90
8200 50 ml 30 ml 12 s 5s 5 min time 90
8.1.1 Perform at least two reagent blank before each batch of samples
8.1.2 Pipette 50 ml of liquid sample or weigh up to 10 g into a 750 ml distillation tube.
In Auto Distillation Units part of this is performed automatically.
8.1.3 Dilute sample with 50 ml H2O.
8.1.4 Add 30 ml of receiver solution to the receiver flask.
8.1.5 Add 30 ml 60 % H3PO4 to the tube.
8.1.6 Set steam pressure to 90 % when using Kjeltec 8100 and 8200
8.1.7 Allow reaction to settle (delay).
8.1.8 Distil for the prescribed time (see below).
8.1.9 Remove sample from the distillation unit and titrate distillate with standardized NaOH.

NOTES:
1. Check recovery rates with sodium sulphite (Na2SO3) as standard.
2. Adjust the sample amount and concentration of titrant according to the sulphite concentration. For very
low concentrations (< 20 mg/L) it is recommended to use 100 to 200 ml sample, adjust the dilution to 0 ml

(T-B) x N x 32 000
_____________________________________
ppm SO2 =
Volume (ml) or weight (g) of sample

T = Volume of titrant for sample (ml)


B = Volume of titrant for blank (ml)
N = Normality of titrant

Recovery: > 90 %
Sample Red wine Beer 1 Beer 2 Dried apricots
Amount 50 ml 50 ml 50 ml 3g
SO2 concentration 202.9 23.0 15.4 1527
(ppm)
215.7 23.7 15.4 1550
211.2 23.7 14.7 1510
214.4 25.0 14.1 1460
213.8 24.3 13.4 1629
202.9 21.8 14.1 1551
209.3 26.2 16.0 1494
Mean SO2 210.0 23.9 14.6 1532
concentration (ppm)
2.5 5.9 6.2 3.5
%RSD
Table 1: Results of samples containing SO2 and relative standard deviations of repeatability (%RSD)

REFERENCES
AOAC 962.16, Sulfurous Acid (Total) in Food
AOAC 990.28, Sulfites in Food
2676/EEC, Commission Regulation of 17 September 1990 Determining Community Methods for the Analysis of
Wine
OIV MA-E-AS323-04-DIOSOU, Compendium of international Methods of Wine and Must Analysis

Revision Description of Change Date Sign


Rev. 5 Up-date for Kjeltec 2000 and 8000 series 2010-01-14 CHg
Method performance data
Indicator Tashiro
Added citric acid
Replaces ASNs 3203, 3204, 3205, 3206, 3207, 3208,
3209, 3210
New template

Rev. 6 Shrimps as a sample type is removed 2011-04-15 HSm