Moisture Measurement in Meat Products by Temperature Controlled

Microwave Drying to a Constant Weight

S. P. Hailey1*, C.R. Moser1, B.J. Haire1, J.T. Keeton2 1CEM Corporation, Matthews, USA; 2Texas A&M University, USA

Steve.Hailey@cem.com

ExperimentComparison of Moisture Determination by

Temperature Controlled Microwave Drying to a Constant Weight with AOAC Convection Oven Reference Method in Meat and Poultry Samples

for NMR Fat Analysis

Participating Laboratories

CEM Corporation (submitting laboratory)

Texas A&M Univ. Meat Science (peer laboratory)

Special thanks to: Dr. Jimmy Keeton & his staff

Apparatus

Moisture DeterminationForced Air Oven Microwave Moisture/Solids Analyzer

Fat DeterminationPetroleum Ether Extraction Equipment Nuclear Magnetic Resonance

Microwave Moisture TestingTare 2 glass fiber sample padsApply sample to pads and press “start”Microwave System: Takes initial sample weight Starts microwaves

• IR Temperature feedback controls microwave power Measures weight loss

• 0.1mg balance Takes final sample weight Displays %Moisture or %Total Solids

SetActual

Magnetron

Infrared Sensor

Microprocessor

Power Control

MicrowaveEnergy

Microwave DryingUsing IR Temperature Control

InfraredData

Smart System 5Smart System 5TMTM

Air ShieldAir Shield

CPUCPU BalanceBalance

IR TemperatureIR TemperatureSensorSensor

Cavity Cavity ExhaustExhaust

MagnetronMagnetron

200200

180180

160160

140140

120120

100100

8080

6060

4040

2020

00

3.53.5

33

2.52.5

22

1.51.5

11

0.50.5

0000 :30:30 1:001:00 1:301:30 2:002:00 2:302:30

TimeTime

IR T

empe

ratu

re

IR T

empe

ratu

re oo CC

Sample W

eight (gms)

Sample W

eight (gms)

Standardize Methods by Controlling Standardize Methods by Controlling Temperature and Monitoring Weight Loss Temperature and Monitoring Weight Loss

During DryingDuring Drying

Temperature Controlled Drying to Constant Weight

Fat Determination on Dried Sample Fat Determination on Dried Sample by by

Nuclear Magnetic Resonance

Why to Dry the Sample In the NMR we are going to cause a energy change in our sample. Force all protons to High Energy State.

Water, Fat, Protein, Carbohydrates

Measure the Free Induction Decay (FID) as the sample reverts or “Relaxes” Back to Equilibrium (low energy state).

Water and Fat have very similar signal

How to Solve Interference of Water with Fat Using spin echo or other techniques in the NMR

OK for low moisture productsMore difficult for high moisture productsRequires up to 20 minuets conditioning in heater block

Dry Sample to Remove WaterConvection oven drying is too slow for process controlIR moisture balance• Slow for high moisture samples • Sample degradation

Microwave Drying• Fastest technique• No sample degradation

Reference Data

MoistureAOAC method 950.46(b) for moisture analysis100 – 102 oC for 16 hours

FatAOAC method 960.39(a) for fat analysisPetroleum ether extraction for 16 hours

Sample Preparation

Approximately 11 kg of freshly processed products from each category were collected.

Diced samples into 5 cm cubes and passed 2 times through Hobart grinder with 4.8mm plate.

Ground meat products were homogenized in Robot Coupe bowl chopper to a paste.

Comparison Data

Data collected on CEM SMART Trac System at Texas A&M

Data collected on CEM SMART Trac System at CEM Corporation

Reference data collected at Texas A&M

BeefAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

Beef #1 Average 75.0975.09 75.4175.41 74.9274.92 4.01 3.99 4.16Range 0.620.62 0.290.29 0.200.20 0.23 0.16 0.18Std. Dev. 0.320.32 0.090.09 0.060.06 0.13 0.05 0.07

Beef #2 Average 67.2967.29 67.9367.93 67.4467.44 11.92 11.97 12.15Range 0.300.30 0.260.26 0.260.26 1.01 0.16 0.20Std. Dev. 0.170.17 0.090.09 0.090.09 0.48 0.05 0.05

Beef #3 Average 45.3845.38 45.3245.32 45.6045.60 39.59 39.57 40.27Range 1.591.59 0.540.54 0.510.51 1.59 0.84 0.53Std. Dev. 1.121.12 0.140.14 0.150.15 0.67 0.28 0.16

Beef #4 Average 27.7627.76 28.1428.14 27.6627.66 63.28 63.34 64.02Range 2.462.46 1.021.02 0.640.64 1.32 1.43 0.48Std. Dev. 1.121.12 0.300.30 0.200.20 0.70 0.41 0.16

PorkAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

Pork #1 Average 73.8573.85 74.6874.68 74.5374.53 3.33 3.35 3.52Range 0.420.42 0.200.20 0.740.74 0.16 0.14 0.20Std. Dev. 0.170.17 0.060.06 0.210.21 0.09 0.04 0.06

Pork #2 Average 65.7165.71 66.2766.27 66.1366.13 14.11 14.36 14.48Range 0.340.34 0.470.47 0.640.64 0.52 0.54 0.40Std. Dev. 0.150.15 0.140.14 0.180.18 0.22 0.16 0.12

Pork #3 Average 50.0150.01 50.3050.30 50.1150.11 33.79 33.94 34.17Range 0.860.86 0.300.30 0.700.70 0.10 0.52 0.41Std. Dev. 0.360.36 0.080.08 0.250.25 0.06 0.15 0.15

TurkeyAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

Turkey #1 Average 74.8374.83 74.5574.55 75.4575.45 2.88 2.93 2.93Range 1.051.05 0.240.24 0.810.81 0.07 0.13 0.16Std. Dev. 0.510.51 0.090.09 0.250.25 0.05 0.04 0.05

Turkey #2 Average 74.5774.57 74.4174.41 73.8473.84 5.89 5.66 5.85Range 1.191.19 0.290.29 0.240.24 0.66 0.07 0.06Std. Dev. 0.560.56 0.050.05 0.090.09 0.11 0.02 0.03

Turkey #3 Average 48.9748.97 47.0447.04 45.7345.73 32.20 32.05 31.05Range 0.370.37 1.011.01 2.182.18 0.23 0.79 1.65Std. Dev. 0.190.19 0.360.36 0.620.62 0.12 0.23 0.50

ChickenAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

Chicken #1 Average 74.8474.84 75.2275.22 74.8774.87 2.59 2.47 2.59Range 1.431.43 0.300.30 0.880.88 0.63 0.21 0.25Std. Dev. 0.200.20 0.160.16 0.250.25 0.27 0.07 0.08

Chicken #2 Average 71.4871.48 71.4471.44 70.7770.77 10.06 9.85 10.73Range 0.010.01 0.290.29 0.230.23 0.07 0.40 0.32Std. Dev. 0.050.05 0.080.08 0.080.08 0.04 0.11 0.09

Chicken #3 Average 52.1152.11 52.8452.84 52.7652.76 36.01 35.97 35.77Range 1.191.19 1.111.11 0.570.57 0.84 0.31 0.22Std. Dev. 0.090.09 0.080.08 0.250.25 0.33 0.02 0.15

Pork SausageAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

Pork Sausage #1 Average 77.3577.35 77.3077.30 77.1677.16 1.30 1.27 1.29Range 0.290.29 0.230.23 0.530.53 0.57 0.14 0.16Std. Dev. 0.150.15 0.090.09 0.160.16 0.30 0.05 0.05

Pork Sausage #2 Average 62.2162.21 62.4062.40 62.5462.54 19.17 18.54 18.41Range 0.570.57 0.340.34 0.590.59 0.64 0.46 0.36Std. Dev. 0.240.24 0.090.09 0.190.19 0.34 0.15 0.12

Pork Sausage #3 Average 52.9852.98 52.9452.94 53.2053.20 31.58 31.55 31.28Range 0.350.35 0.270.27 0.490.49 0.74 0.61 0.68Std. Dev. 0.180.18 0.080.08 0.170.17 0.30 0.19 0.23

Pork Sausage #4 Average 46.8246.82 46.6246.62 46.5046.50 39.22 39.24 39.15Range 0.650.65 0.430.43 0.360.36 0.54 0.65 0.45Std. Dev. 0.280.28 0.130.13 0.120.12 0.25 0.21 0.14

Cooked SausageAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

Hot Dogs #1 Average 75.6875.68 75.1675.16 75.1675.16 0.53 0.52 0.72Range 0.550.55 0.450.45 0.490.49 0.01 0.20 0.34Std. Dev. 0.330.33 0.160.16 0.190.19 0.01 0.06 0.11

Hot Dogs #2 Average 64.4664.46 64.6664.66 63.8363.83 15.83 15.40 16.09Range 0.450.45 0.380.38 0.440.44 0.97 0.39 0.41Std. Dev. 0.210.21 0.120.12 0.150.15 0.51 0.12 0.13

Hot Dogs #3 Average 52.5652.56 52.4352.43 52.1152.11 30.75 30.73 30.93Range 1.041.04 0.190.19 0.400.40 0.66 0.57 0.35Std. Dev. 0.430.43 0.050.05 0.140.14 0.32 0.17 0.14

HamAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

Ham #1 Average 75.9675.96 76.4576.45 76.7176.71 2.11 2.04 2.10Range 0.550.55 0.190.19 0.710.71 0.32 0.13 0.22Std. Dev. 0.270.27 0.070.07 0.210.21 0.23 0.05 0.07

Ham #2 Average 73.5073.50 73.5073.50 73.3873.38 2.52 2.57 2.63Range 0.300.30 0.240.24 0.780.78 0.30 0.09 0.26Std. Dev. 0.130.13 0.080.08 0.260.26 0.15 0.02 0.08

Ham #3 Average 55.5155.51 54.9654.96 54.0854.08 20.59 20.57 21.43Range 0.780.78 0.690.69 0.350.35 0.72 0.59 0.17Std. Dev. 0.320.32 0.240.24 0.100.10 0.33 0.20 0.06

Ham #4 Average 65.6865.68 65.4665.46 65.3365.33 10.51 10.53 10.65Range 0.390.39 0.180.18 0.550.55 0.06 0.20 0.32Std. Dev. 0.160.16 0.050.05 0.150.15 0.04 0.08 0.09

Beef, fresh ground , high fatAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

12345678910

MeanSD

40.4440.4440.4240.4240.3540.3540.2640.2640.4940.4940.3440.3440.4140.4140.4440.4440.3040.3040.4540.45

40.3940.390.0740.074

40.1940.1940.1340.1340.2640.2640.2040.2040.1940.1940.3540.3540.4440.4440.3340.3340.3640.3640.3240.32

40.2840.280.0980.098

40.6940.6940.2340.2340.1840.1840.6840.6840.2440.2440.3240.3240.4240.4240.3940.3940.4240.4240.5940.59

40.4240.420.1840.184

46.0345.8645.8345.5445.9245.7345.6445.9245.9345.99

45.840.157

46.3446.1546.0846.2546.1945.9945.5945.6545.5045.87

45.960.295

45.6846.2546.2745.9346.2446.4045.9445.9245.8545.54

46.000.280

Chicken, fresh with skinAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

12345678910

MeanSD

74.5274.5274.5674.5674.5974.5974.5574.5574.5274.5274.6074.6074.6074.6074.5874.5874.6474.6474.5674.56

74.5774.570.0380.038

74.5574.5574.5174.5174.6674.6674.6574.6574.5374.5374.4274.4274.6574.6574.2574.2574.2574.2574.3174.31

74.4874.480.1620.162

74.2874.2874.2374.2374.3874.3874.1874.1874.3274.3274.4274.4274.5574.5574.4074.4074.4174.4174.5474.54

74.3774.370.1210.121

7.367.507.027.497.087.067.167.087.417.20

7.240.186

7.257.347.337.327.297.267.247.257.307.27

7.290.036

7.297.147.227.217.087.167.077.107.077.11

7.150.074

NIST SRM 1546AOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

12345678910

MeanSD

59.3759.3759.5459.5459.4159.4159.3859.3859.5359.5359.2459.2459.4159.4159.4959.4959.1559.1558.9858.98

59.3559.350.1780.178

58.6458.6458.4458.4458.4558.4558.5358.5358.3158.3158.5958.5958.4158.4158.4758.4758.5458.5458.4458.44

58.4858.480.0950.095

59.2459.2458.9058.9058.7658.7658.7358.7358.9258.9258.7358.7359.0259.0258.7758.7758.7058.7058.5358.53

58.8658.860.2050.205

21.6921.6921.7121.3721.5821.3221.1421.9321.9921.94

21.640.286

21.7721.7621.6221.6021.7921.5821.7121.6121.5621.48

21.650.104

20.9721.1320.9120.5220.9420.9820.6221.0820.7321.11

20.900.207

Note: Three different cans of NIST material were used for the above results.NIST Reference Values: Moisture 59.5% +/-2.6%; fat value 21.0% +/-1.4%

All Beef Hot DogsAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

12345678910

MeanSD

51.5151.5151.4551.4551.6451.6451.5451.5451.6351.6351.7551.7551.8751.8751.8951.8951.8051.8051.6951.69

51.6851.680.1520.152

51.5551.5551.4251.4251.6451.6451.5351.5351.4651.4651.4751.4751.3851.3851.2651.2651.4451.4451.1751.17

51.4351.430.1380.138

51.7951.7951.9651.9651.5851.5851.5951.5951.9751.9751.4751.4751.6651.6651.9751.9751.6951.6951.4951.49

51.7251.720.1950.195

30.5930.6130.4430.5330.6330.3630.7230.2030.5430.18

30.480.183

30.6330.6430.2830.4630.6530.3630.7230.5730.4230.71

30.540.154

30.3030.7730.6030.2930.3630.6330.4530.4030.6330.71

30.510.175

Pork, fresh, low fatAOACAOAC CEMCEM TAMTAM AOAC CEM TAM

Sample ID %M%M %M %M %M %M %F %F %F

12345678910

MeanSD

73.9073.9073.9173.9173.8373.8373.9373.9374.0674.0674.0374.0374.0074.0074.0274.0273.9273.9273.8073.80

73.9473.940.0870.087

73.9073.9073.7973.7973.7473.7473.6073.6073.7773.7773.7473.7473.6673.6673.7073.7073.7373.7373.5873.58

73.7273.720.0940.094

73.6573.6573.7673.7673.7273.7273.8873.8873.7373.7373.6973.6973.8173.8173.4673.4674.0074.0073.7573.75

73.7573.750.1420.142

3.753.863.443.693.843.953.763.783.583.78

3.740.146

3.753.743.773.783.783.773.793.743.743.77

3.760.019

3.773.853.943.873.923.933.804.053.793.85

3.880.085

SummarySummaryAOAC Methods for Moisture in Meat by Microwave Drying AOAC Methods for Moisture in Meat by Microwave Drying

Official Method 985.14 final action 1991Official Method 985.14 final action 1991Peer Verified Method PVM1:2003, issued 2003Peer Verified Method PVM1:2003, issued 2003

Temperature Controlled Microwave Drying Temperature Controlled Microwave Drying Allows method transfer to different instruments without adjustment of drying Allows method transfer to different instruments without adjustment of drying programprogramAvoids heat degradation of sampleAvoids heat degradation of sample• Dried sample available for NMR fat determinationDried sample available for NMR fat determination

Sample is automatically temperature conditioned for NMRSample is automatically temperature conditioned for NMR• Avoids temperature conditioning in heater blockAvoids temperature conditioning in heater block

Constant Weight DryingConstant Weight DryingClassical method for weight loss on drying determinationClassical method for weight loss on drying determinationAssures moisture is removed from sampleAssures moisture is removed from sampleOptimized drying timeOptimized drying time