Don't be fooled - getting the same result twice with expensive equipment does not mean the answer is reliable!

Don't be Fooled - Malic Acid Testing

 

I recently attended the Unified Wine & Grape Symposium in Sacramento.  A few winemakers I spoke with asked about the precision of the Accuvin Malic Acid test kit.  As has been reported, the accuracy of the Malic Acid test kit is +/- 10 mg/L at the 30 mg/L level, which is generally considered the end of MLF, and about +/- 20 mg/L at the 75 mg/L level.

 

These questions reminded me of the of the Wine Industry Interlaboratory Testing Program that has be going on since 1999.1,2,3  The program, set up by the ASEV and UC Davis, is meant to help winery labs improve the quality of their results.  In this program, two wine samples are sent out a few times a year to the 40 – 55 participating winery labs.  The samples are analyzed at least in duplicate, and the results are sent back for statistical analysis.  The most common method used by far was enzymatic.  A table of the results is given below for wine samples with malic acid levels below 500 mg/L.  From 10% to 23% of the results were found to be unreliably inaccurate, and are not included in the table.

 

(Data from the Wine Industry Interlaboratory Testing Program)

 

 

 

Sample 1

 

 

Year

Season

Sample

mean

sd

95% confidence

cv

actual range

samples

 

 

No.

 

 

interval

 

reported

discarded

1999

Summer

1

100

19

63 - 137

19.0

 

no.

%

2000

Summer

3A

440

54

334 - 546

12.3

 

 

 

2000

Summer

3B

210

47

118 - 302

22.5

 

 

 

2000

Fall

4

180

54

74 - 286

29.8

 

 

 

2000

Winter

5

160

55

52 - 268

34.2

 

 

 

2003

Fall

15A

96

24

49 - 143

25.0

35 - 160

4/37

11

2003

Fall

15B

103

34

36 - 170

33.0

35 - 175

4/37

11

2004

Summer

17A

165

44

79 - 251

26.7

66 - 277

4/43

9

2004

Summer

17B

118

42

36 - 200

35.6

15 - 225

4/43

9

2005

Spring

19A

112

43

28 - 196

38.4

25 - 230

5/47

11

2005

Spring

19B

135

41

55 - 215

30.4

50 - 240

5/47

11

2005

Fall

21A

165

56

55 - 275

33.9

11 - 300

5/49

10

2005

Fall

21B

163

54

57 - 269

33.1

17 - 300

5/49

10

2006

Summer

23A

275

34

208 - 342

12.4

210 - 351

6/44

14

2006

Summer

23B

176

34

109 - 243

19.3

120 - 260

6/44

14

2007

Summer

26A

218

76

69 - 367

34.9

125 - 450

8/51

16

2007

Summer

26B

110

62

0 - 232

56.4

30 - 300

8/51

16

2008

Summer

29A

98

41

18 - 178

41.8

8 - 210

13/57

23

2008

Summer

29B

99

41

19 - 179

41.4

3 - 219

13/57

23

 

 

 

 

 

 

 

 

 

 

 

What do these results show?

 

First, in the nine years the quality improvement program has been going on, the results have gotten progressively worse.  The coefficient of variation, a measure of lab to lab reproducibility, has doubled.  In addition, while in the initial years 10% of the reported results were so far off the mark that they had to be excluded, the number of totally unusable results climbed to 23% in the latest report.

 

Second, the results have deteriorated to the point where about half are flat out wrong regarding what they tell the winemaker.  In 1999, a sample with a malic acid level of 100 mg/L was analyzed, with the results showing a range of 63 – 137 mg/L.  That’s pretty broad.  In 2007 a wine with a malic acid level of 110 mg/L was analyzed, and the results ranged from 30 – 200 mg/L.  In 2008 a sample with a malic acid level of 96 mg/L was analyzed, and the range for the results had ballooned to 18 – 178 mg/L.  Some winemakers were told their wines had finished MLF (which they hadn’t), while other winemakers thought they had a few weeks yet to go (which they didn’t).  And remember, that huge range was the range reported AFTER 23% of the results had been discarded for gross unreliability.  (By the way, if an Accuvin test strip had been used to analyze the above samples, you could expect the results to be in the range of 75 – 125 mg/L.  That’s considerably better!)

 

In 2002 Dr. Christian Butzke of UC Davis wrote a critique of the first few years of the program.  Regarding malic acid he wrote:  “Given the corresponding consequences of uncertainty over incomplete or deliberately prevented malolactic fermentation, in particular CO2 evolution in the bottle and changes in perceived acidity, this performance requires major improvements.”1 What would he say today?

 

Don’t be fooled!  Spending money on expensive equipment or excessive time running laboratory tests does not ensure reliable results.

 

What are typical results you can expect?

 

Actual Value

Expected Range

 

 

 

Accuvin

98

73 - 123

per the QC Survey

98

18 - 178

 

 

 

Accuvin

96

71 - 121

per the QC Survey

96

49 - 143

 

 

 

Accuvin

112

87 - 137

per the QC Survey

112

26 - 196

 

 

 

Accuvin

118

93 - 143

per the QC Survey

118

36 - 200

 

 

 

Accuvin

103

78 - 128

per the QC Survey

103

36 - 170

 

 

 

Accuvin

110

85 - 135

per the QC Survey

110

0 - 232

 

 

A final thought:  just getting the same answer twice with a method performed unreliably does not make it the correct answer.

 

1   C. E. Butzke, Am. J. Enol. Vitic., 53 (20: 163 – 169 ) 2002.

2   C. E. Butzke, Practical  Winery & Vineyard, Jan. Feb. 2002

3   Collaborative Testing Services, Inc., www.cts-interlab.com/wine/index.html, reports, 2003 - 2008

 

What did you think of this article?




Trackbacks
  • No trackbacks exist for this post.
Comments
  • No comments exist for this post.
Leave a comment

Submitted comments are subject to moderation before being displayed.

 Enter the above security code (required)

 Name

 Email (will not be published)

 Website

Your comment is 0 characters limited to 3000 characters.