moisture measurement in meat products by temperature controlled microwave drying to a constant...
TRANSCRIPT
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
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 Determination
Forced Air Oven
Microwave Moisture/Solids Analyzer
Fat Determination
Petroleum Ether Extraction Equipment
Nuclear Magnetic Resonance
Microwave Moisture TestingTare 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
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
emp
erat
ure
IR
Tem
per
atu
re oo CC
Sam
ple W
eight (gm
s)S
amp
le Weigh
t (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
Moisture
AOAC method 950.46(b) for moisture analysis
100 – 102 oC for 16 hours
Fat
AOAC method 960.39(a) for fat analysis
Petroleum 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