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Moisture Measurement in Meat Products by Temperature Controlled Microwave Drying to a Constant Weight S. P. Hailey 1*, C.R. Moser 1, B.J. Haire 1, J.T.

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Presentation on theme: "Moisture Measurement in Meat Products by Temperature Controlled Microwave Drying to a Constant Weight S. P. Hailey 1*, C.R. Moser 1, B.J. Haire 1, J.T."— Presentation transcript:

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2 Moisture Measurement in Meat Products by Temperature Controlled Microwave Drying to a Constant Weight S. P. Hailey 1*, C.R. Moser 1, B.J. Haire 1, J.T. Keeton 2 1 CEM Corporation, Matthews, USA; 2 Texas A&M University, USA Steve.Hailey@cem.com Steve.Hailey@cem.com

3 Experiment Comparison 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

4 Participating Laboratories CEM Corporation (submitting laboratory) Texas A&M Univ. Meat Science (peer laboratory) Special thanks to: Dr. Jimmy Keeton & his staff

5 Apparatus Moisture Determination Forced Air Oven Microwave Moisture/Solids Analyzer Fat Determination Petroleum Ether Extraction Equipment Nuclear Magnetic Resonance

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7 Microwave Moisture Testing Tare 2 glass fiber sample pads Apply 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

8 SetActual Magnetron Infrared Sensor Microprocessor Power Control Microwave Energy Microwave Drying Using IR Temperature Control Infrared Data

9 Smart System 5 TM Air Shield CPU Balance IR Temperature Sensor CavityExhaust Magnetron

10 200180160140120100806040200 3.532.521.510.50 0:301:001:302:002:30 Time IR Temperature o C Sample Weight (gms) Standardize Methods by Controlling Temperature and Monitoring Weight Loss During Drying Temperature Controlled Drying to Constant Weight

11 Fat Determination on Dried Sample by Fat Determination on Dried Sample by N uclear M agnetic R esonance

12 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

13 How to Solve Interference of Water with Fat Using spin echo or other techniques in the NMR OK for low moisture products More difficult for high moisture products Requires up to 20 minuets conditioning in heater block Dry Sample to Remove Water Convection oven drying is too slow for process control IR moisture balance Slow for high moisture samples Sample degradation Microwave Drying Fastest technique No sample degradation

14 Reference Data Moisture AOAC method 950.46(b) for moisture analysis 100 – 102 o C for 16 hours Fat AOAC method 960.39(a) for fat analysis Petroleum ether extraction for 16 hours

15 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.

16 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

17 Beef AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 75.0975.4174.92 Beef #1Average75.0975.4174.924.013.994.16 0.620.290.20 Range0.620.290.200.230.160.18 0.320.090.06 Std. Dev.0.320.090.060.130.050.07 67.2967.9367.44 Beef #2Average67.2967.9367.4411.9211.9712.15 0.300.260.26 Range0.300.260.261.010.160.20 0.170.090.09 Std. Dev.0.170.090.090.480.050.05 45.3845.3245.60 Beef #3Average45.3845.3245.6039.5939.5740.27 1.590.540.51 Range1.590.540.511.590.840.53 1.120.140.15 Std. Dev.1.120.140.150.670.280.16 27.7628.1427.66 Beef #4Average27.7628.1427.6663.2863.3464.02 2.461.020.64 Range2.461.020.641.321.430.48 1.120.300.20 Std. Dev.1.120.300.200.700.410.16

18 Pork AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 73.8574.6874.53 Pork #1Average73.8574.6874.533.333.353.52 0.420.200.74 Range0.420.200.740.160.140.20 0.170.060.21 Std. Dev.0.170.060.210.090.040.06 65.7166.2766.13 Pork #2Average65.7166.2766.1314.1114.3614.48 0.340.470.64 Range0.340.470.640.520.540.40 0.150.140.18 Std. Dev.0.150.140.180.220.160.12 50.0150.3050.11 Pork #3Average50.0150.3050.1133.7933.9434.17 0.860.300.70 Range0.860.300.700.100.520.41 0.360.080.25 Std. Dev.0.360.080.250.060.150.15

19 Turkey AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 74.8374.5575.45 Turkey #1Average74.8374.5575.452.882.932.93 1.050.240.81 Range1.050.240.810.070.130.16 0.510.090.25 Std. Dev.0.510.090.250.050.040.05 74.5774.4173.84 Turkey #2Average74.5774.4173.845.895.665.85 1.190.290.24 Range1.190.290.240.660.070.06 0.560.050.09 Std. Dev.0.560.050.090.110.020.03 48.9747.0445.73 Turkey #3Average48.9747.0445.7332.2032.0531.05 0.371.012.18 Range0.371.012.180.230.791.65 0.190.360.62 Std. Dev.0.190.360.620.120.230.50

20 Chicken AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 74.8475.2274.87 Chicken #1Average74.8475.2274.872.592.472.59 1.430.300.88 Range1.430.300.880.630.210.25 0.200.160.25 Std. Dev.0.200.160.250.270.070.08 71.4871.4470.77 Chicken #2Average71.4871.4470.7710.069.8510.73 0.010.290.23 Range0.010.290.230.070.400.32 0.050.080.08 Std. Dev.0.050.080.080.040.110.09 52.1152.8452.76 Chicken #3Average 52.1152.8452.7636.0135.9735.77 1.191.110.57 Range1.191.110.570.840.310.22 0.090.080.25 Std. Dev.0.090.080.250.330.020.15

21 Pork Sausage AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 77.3577.3077.16 Pork Sausage #1Average77.3577.3077.161.301.271.29 0.290.230.53 Range0.290.230.530.570.140.16 0.150.090.16 Std. Dev.0.150.090.160.300.050.05 62.2162.4062.54 Pork Sausage #2Average62.2162.4062.5419.1718.5418.41 0.570.340.59 Range0.570.340.590.640.460.36 0.240.090.19 Std. Dev.0.240.090.190.340.150.12 52.9852.9453.20 Pork Sausage #3Average52.9852.9453.2031.5831.5531.28 0.350.270.49 Range0.350.270.490.740.610.68 0.180.080.17 Std. Dev.0.180.080.170.300.190.23 46.8246.6246.50 Pork Sausage #4Average46.8246.6246.5039.2239.2439.15 0.650.430.36 Range0.650.430.360.540.650.45 0.280.130.12 Std. Dev.0.280.130.120.250.210.14

22 Cooked Sausage AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 75.6875.1675.16 Hot Dogs #1Average75.6875.1675.160.530.520.72 0.550.450.49 Range0.550.450.490.010.200.34 0.330.160.19 Std. Dev.0.330.160.190.010.060.11 64.4664.6663.83 Hot Dogs #2Average64.4664.6663.8315.8315.4016.09 0.450.380.44 Range0.450.380.440.970.390.41 0.210.120.15 Std. Dev.0.210.120.150.510.120.13 52.5652.4352.11 Hot Dogs #3Average52.5652.4352.1130.7530.7330.93 1.040.190.40 Range1.040.190.400.660.570.35 0.430.050.14 Std. Dev.0.430.050.140.320.170.14

23 Ham AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 75.9676.4576.71 Ham #1Average75.9676.4576.712.112.042.10 0.550.190.71 Range0.550.190.710.320.130.22 0.270.070.21 Std. Dev.0.270.070.210.230.050.07 73.5073.5073.38 Ham #2Average73.5073.5073.382.522.572.63 0.300.240.78 Range0.300.240.780.300.090.26 0.130.080.26 Std. Dev.0.130.080.260.150.020.08 55.5154.9654.08 Ham #3Average55.5154.9654.0820.5920.5721.43 0.780.690.35 Range0.780.690.350.720.590.17 0.320.240.10 Std. Dev.0.320.240.100.330.200.06 65.6865.4665.33 Ham #4Average65.6865.4665.3310.5110.5310.65 0.390.180.55 Range0.390.180.550.060.200.32 0.160.050.15 Std. Dev.0.160.050.150.040.080.09

24 Beef, fresh ground, high fat AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 1 2 3 4 5 6 7 8 9 10 Mean SD 40.4440.4240.3540.2640.4940.3440.4140.4440.3040.4540.390.074 40.1940.1340.2640.2040.1940.3540.4440.3340.3640.3240.280.098 40.6940.2340.1840.6840.2440.3240.4240.3940.4240.5940.420.184 46.03 45.86 45.83 45.54 45.92 45.73 45.64 45.92 45.93 45.99 45.84 0.157 46.34 46.15 46.08 46.25 46.19 45.99 45.59 45.65 45.50 45.87 45.96 0.295 45.68 46.25 46.27 45.93 46.24 46.40 45.94 45.92 45.85 45.54 46.00 0.280

25 Chicken, fresh with skin AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 1 2 3 4 5 6 7 8 9 10 Mean SD 74.5274.5674.5974.5574.5274.6074.6074.5874.6474.5674.570.038 74.5574.5174.6674.6574.5374.4274.6574.2574.2574.3174.480.162 74.2874.2374.3874.1874.3274.4274.5574.4074.4174.5474.370.121 7.36 7.50 7.02 7.49 7.08 7.06 7.16 7.08 7.41 7.20 7.24 0.186 7.25 7.34 7.33 7.32 7.29 7.26 7.24 7.25 7.30 7.27 7.29 0.036 7.29 7.14 7.22 7.21 7.08 7.16 7.07 7.10 7.07 7.11 7.15 0.074

26 NIST SRM 1546 AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 1 2 3 4 5 6 7 8 9 10 Mean SD 59.3759.5459.4159.3859.5359.2459.4159.4959.1558.9859.350.178 58.6458.4458.4558.5358.3158.5958.4158.4758.5458.4458.480.095 59.2458.9058.7658.7358.9258.7359.0258.7758.7058.5358.860.205 21.69 21.71 21.37 21.58 21.32 21.14 21.93 21.99 21.94 21.64 0.286 21.77 21.76 21.62 21.60 21.79 21.58 21.71 21.61 21.56 21.48 21.65 0.104 20.97 21.13 20.91 20.52 20.94 20.98 20.62 21.08 20.73 21.11 20.90 0.207 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%

27 All Beef Hot Dogs AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 1 2 3 4 5 6 7 8 9 10 Mean SD 51.5151.4551.6451.5451.6351.7551.8751.8951.8051.6951.680.152 51.5551.4251.6451.5351.4651.4751.3851.2651.4451.1751.430.138 51.7951.9651.5851.5951.9751.4751.6651.9751.6951.4951.720.195 30.59 30.61 30.44 30.53 30.63 30.36 30.72 30.20 30.54 30.18 30.48 0.183 30.63 30.64 30.28 30.46 30.65 30.36 30.72 30.57 30.42 30.71 30.54 0.154 30.30 30.77 30.60 30.29 30.36 30.63 30.45 30.40 30.63 30.71 30.51 0.175

28 Pork, fresh, low fat AOACCEMTAM AOACCEMTAMAOACCEMTAM %M %M %M Sample ID%M %M %M %F %F %F 1 2 3 4 5 6 7 8 9 10 Mean SD 73.9073.9173.8373.9374.0674.0374.0074.0273.9273.8073.940.087 73.9073.7973.7473.6073.7773.7473.6673.7073.7373.5873.720.094 73.6573.7673.7273.8873.7373.6973.8173.4674.0073.7573.750.142 3.75 3.86 3.44 3.69 3.84 3.95 3.76 3.78 3.58 3.78 3.74 0.146 3.75 3.74 3.77 3.78 3.77 3.79 3.74 3.77 3.76 0.019 3.77 3.85 3.94 3.87 3.92 3.93 3.80 4.05 3.79 3.85 3.88 0.085

29 Summary AOAC Methods for Moisture in Meat by Microwave Drying Official Method 985.14 final action 1991 Peer Verified Method PVM1:2003, issued 2003 Temperature Controlled Microwave Drying Allows method transfer to different instruments without adjustment of drying program Avoids heat degradation of sample Dried sample available for NMR fat determination Dried sample available for NMR fat determination Sample is automatically temperature conditioned for NMR Avoids temperature conditioning in heater block Avoids temperature conditioning in heater block Constant Weight Drying Classical method for weight loss on drying determination Assures moisture is removed from sample Optimized drying time

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