Table I
Correlation of source factors in quantitative spectrographic analysis.
Precision Sensitivity Range Influence of one element on another Arc-like source Electrode phenomena Low because of erratic wandering of arc and erratic conduction of heat away from the tip Large amount of material contributed to discharge High because of effect of varying amounts of elements on fractional distillation process Arc-like source Discharge phenomena Should be capable of high precision High because of high concentration of material in discharge and high absolute sensitivity of arc lines Limited by self-absorption High because of high concentration of material compared to the amount of energy available for excitation Spark-like source Electrode phenomena High because many hundred portions are sampled for each exposure Small amount of material contributed to discharge Little because fractional distillation as such has little to do with getting the sample into the discharge Spark-like source Discharge phenomena High if each spark is controlled so that the total is a summation of identical discharges Low because of low concentration of material in discharge and many sensitive spark lines are in the vacuum region Limited by low sensitivity Little because of low concentration of material and large amount of energy available
Table II
Standard and special conditions used in the analysis of metals with the controlled multisource.
Spectrograph: Applied Research Labs. —Dietert grating spectrograph, 2360–4580A region. Sample form: disks 7/32″ rods Cooling: none cooled during exposure Upper electrode: sample sample (150° truncated cone) Densitometer: Applied Research Labs. —Dietert projection-comparator densitometer. Lower electrode: National Carbon Co. sample (150° truncated cone) Special graphite Spectroscopic electrodes
1
4
″ Source: Applied Research Labs.— Dietert controlled multisource Analytical gap: 2 mm 3 mm Peak voltage, secondary power circuit: 940 volts Apertures: One at secondary focus and a second one-half inch in front of analytical gap (0.060″) One 0.060″ at secondary focus Slit: 60 microns Lens: none Film: Special Eastman Experimental Spectrum No. 2 Developer: D19 Development conditions: 3 minutes at 70°F Contrast: 1.2–1.3 Calibration: calibrated iron spectrum given the same exposure time as samples
Material Capacitance (microfarads) Inductance (microhenries) Resistance (ohms) Pre-exposure discharge time (sec.) Exposure time (sec.) Exposures per spectrum Lower electrode Circuit Discharge type Fe (rods) 2 50 0.4 10 30 1 oscillating spark-like Fe (disks) 4 180 10 10 30 1 120° cone oscillating spark-like Cu, Fe, Mg 5 100 10 10 30 1 120° cone critically damped spark-like Zn (disks) Al, Fe, Mg Zn (disks) 5 480 100 10 30 1 120° cone overdamped spark-like Cu (disks) 5 480 100 30 30 1 120° cone overdamped spark-like Fe (rods)* 40 480 50 3 10 1 overdamped arc-like Fe (disks) 40 480 50 3 5 2 120° cone overdamped arc-like Al, Mg, Cu (disks) 60 480 50 3 5 2 20° cone overdamped arc-like Zn (disks)** 60 480 50 0 5 1 20° cone overdamped arc-like
* Upper electrode negative, positive in all other cases.
** Sample in form of raised 60° cone on surface of sample.
Table III
Data for the analysis of steel rods.
Range Sensitivity (I =0.3 background) Line pair Working curve linear at 45° Working curve self-absorbed Index point* Precision (% average deviation) a. c =2 μ f, L =50 μ h, R =0.4 ohm. Ni 3414.8 0.04% 3414.8/3009.6 0.1 –1.5% 1.38% 1.1% Cr 4254.3 0.03 2822.4/3009.6 0.13 –2.8% 0.79 1.4 Mn 2576.1 0.01 2933.1/3009.6 0.2 –1.5 0.385 1.6 Mo 3684.1 0.02 2816.2/3009.6 0.14 –1.2 0.43 2816.2 0.04 Si 2881.6 0.05 2881.6/3009.6 0.12 –0.43 1.7 V 4379.2 0.06 3102.3/3009.6 0.025 –0.30 0.175 1.4 3093.1 0.004 Cu 3274.0 0.004 3274.0/3009.6 0.015–0.22 1.4 b. C =40 μ f, L =480 μ h, R =50 ohms. Ni 3414.8 0.002% 3414.8/3200.5 0.004 –0.2% 0.2 –3.0% 0.38% 2.6% Cr 4254.3 0.0008 2677.2/2506.1 0.011 –0.15 0.15 –2.7 0.415 2.4 Mn 2576.1 0.004 4041.4/4216.2 0.25 –1.6 0.325 1.5 Mo 3684.1 0.002 2816.2/3200.5 0.02 –0.1 0.1 –1.0 2816.2 0.01 Si 2881.6 0.003 2881.6/3200.5 0.013 –0.44 0.39 1.2 V 4379.2 0.003 4379.2/4375.9 0.0025–0.27 0.19 2.3 3093.1 0.002 Cu 3274.0 0.0002 3274.0/3200.5 0.018 –0.21 0.305
* Percent at which the intensity ratio of the line pair given is equal to one.
Table IV
Data for the analysis of steel disks.
Range Sensitivity (I =0.3 background) Line pair Working curve linear at 45° Working curve self-absorbed Index point* Precision (% average deviation) a. C =4 μ f, L =480 μ h, R =10 ohms. Ni 3414.8 0.01% 3493.0/3009.6 0.1 –1.3% Cr 4254.3 0.01 2822.4/2823/3 0.1 –1.0% 1.0 –2.8 1.2% 1.3% Mn 4030.8 0.02 2933.1/3009.6 0.21 –0.6 0.6 –1.8 0.36 0.29 2576.1 0.01 Mo 2816.2 0.01 2816.2/3009.6 0.045–1.0 Si 2881.6 0.02 2881.6/3009.6 0.011–0.5 1.5 V 3093.1 0.01 3093.1/3009.6 0.028–0.32 0.263 1.3 Cu 3274.0 0.002 3274.0/3009.6 0.013–0.26 2.0 b. C =5 μ f, L =480 μ h, R =100 ohms. Ni 3414.8 0.06% 3414.8/3009.6 0.1 –3.6% 1.6% 1.3% Cr 4254.3 0.02 2822.4/3009.6 0.16 –3.0% 1.15 0.99 Mn 4030.8 0.04 4034.5/3009.6 0.2 –1.7 0.98 1.0 Mo 2816.2 0.02 2816.2/3009.6 0.054–1.0 0.85 1.4 Si 2881.6 0.02 2881.6/3009.6 0.011–0.06 0.06 –0.4 1.7 V 4379.2 0.03 3093.1/3009.6 0.034–0.3 0.155 1.9 3093.1 0.006 Cu 3274.0 0.003 3274.0/3009.6 0.012–0.25 0.137 2.5 c. C =40 μ f, L =480 μ h, R =50 ohms. Ni 3414.8 0.006% 3414.8/3009.6 0.053–0.5% 0.5 –4.2% 1.62% 1.7% Cr 4254.3 0.002 2677.2/3009.6 0.014–0.3 0.3 –5.0 1.04 2.4 Mn 4034.5/3009.6 0.13 –2.0 0.58 2.9 Si 2881.6 0.003 2881.6/3009.6 0.012–0.2 3.6 V 4379.2 0.007 3093.1/3009.6 0.053–0.27 3093.1 0.004 Cu 3274.0 0.006 3274.0/3009.6 0.015–0.3 0.415 Mo 2816.2/3009.6 0.1 –1.1
* Percent at which the intensity ratio of the line pair given is equal to one.
Table V
Data for the analysis of aluminum alloys.
Range Sensitivity (I =0.3 background) Line pair Working curve linear at 45° Working curve self-absorbed Index point* Precision (% average deviation) a. C =5 μ f, L =480 μ h, R =100 ohms. Cu 3274.0 0.01% 3274.0/3059.9 0.014 –0.092% 0.0345% 1.2% 2961.2/3059.9 0.8 –5.3 Si 2514.3/3059.9 0.045–4.0% 0.71 1.4 Mg 2852.1 0.001 2852.1/3059.9 0.004 –0.025 0.0076 2783.0/3059.9 0.22 –1.6 1.03 0.59 Mn 2949.2/3059.9 0.003 –0.06 0.06 0.72 2688.2/3059.9 0.4 –1.1 0.87 Fe 3020.6 0.05 2395.6/3059.9 0.08 –0.42 0.163 1.7 Cr 4254.3 0.008 2822.4/3059.9 0.011 –0.044 0.0385 1.2 Sn 3175.1 0.02 3175.0/3059.9 0.02 –0.1 Zn 3345.0 0.04 Ni 3414.8 0.02 3414.8/3059.9 0.01 –0.064 0.66 Mo 3170.3 0.02 3170.3/3059.9 0.0072–0.053 0.047 2.8 Ti 3372.8 0.007 3372.8/3059.9 0.0072–0.054 1.3 b. C =60 μ f, L =480 μ h, R =50 ohms. Cu 3247.5 0.0002% 2824.4/3059.9 0.072 –5.0% 0.52% 1.8% Si 2881.6 0.0005 2435.2/2669.2 0.032 –0.8 0.8 –6.0% 0.36 1.8 Mg 2852.1 0.00007 2779.8/2669.2 0.007 –2.0 0.052 3.4 Mn 4030.8 0.0007 4030.8/2378.4 0.0027–0.032 0.032 2.1 3256.1/3059.9 0.028 –1.0 0.26 Fe 3020.6 0.002 2973.2/2669.2 0.086 –0.72 0.116 1.2 Cr 3021.6/2378.4 0.031 –0.46 0.278 1.8 Sn 3175.0 0.001 3175.0/2378.4 0.013 –0.084 Zn 3345.0 0.002 3345.0/2669.2 0.007 –0.088 0.04 2.1 Ni 3414.8 0.0004 3414.8/2669.2 0.007 –0.065 0.0099 2.7 Mo 3170.3 0.001 3170.2/2669.2 0.01 –0.062 0.0225 2.1 Ti 3372.8 0.001 3372.8/3059.9 0.007 –0.078 0.0233 0.60 Pb 2833.1 0.003
* Percent at which the intensity ratio of the line pair given is equal to one.
Table VI
Data for the analysis of magnesium alloys.
Range Sensitivity (I =0.3 background) Line pair Working curve linear at 45° Working curve self-absorbed Index point* Precision (% average deviation) a. C =5 μ f, L =100 μ h, R =10 ohms. Al 2652.5/3074.0 3.4 –14.5% 12.5% 1.2% Zn 3282.3/3329.9 0.72 – 4.2 0.66 Mn 4030.8 0.01% 2949.2/3329.9 0.067 – 0.46 0.153 1.6 Cu 3274.0 0.002 3274.0/3329.9 0.015 –0.11 0.079 1.1 Si 2881.6 0.03 2881.6/3329.9 0.029 – 0.1 Ni 3414.8 0.007 b. C =60 μ f, L =480 μ h, R =50 ohms. Al 2652.5/3074.0 3.6 –14.5%** 12.3% 1.6% Zn 3282.3/3074.0 0.63 – 5.8 1.03 1.8 Mn 3228.1/3074.0 0.063 –0.59 0.455 3.1 Cu 3274.0/3074.0 0.018 – 0.074 2.5 Si 2881.6 0.02% 2881.6/3074.0 0.019 – 0.073 3.6 Ni 3414.8 0.002 3414.8/3074.0 0.0025– 0.008 Fe 3020.6 0.001 3020.6/3074.0 0.0064– 0.033 1.7 2395.6 0.001
* Percent at which the intensity ratio of the line pair given is equal to one.
** Linear but not at 45°. See
Fig. 4 and text.
Table VII
Data for the analysis of zinc alloys.
Range Sensitivity (I =0.3 background) Line pair Working curve linear at 45° Working curve self-absorbed Index point* Precision (% average deviation) a. C =5 μ f, L =480 μ h, R =100 ohms. Al 2660.4/3018.4 3.0 –7.4% 1.2% Cu 3274.0 0.01% 3274.0/3018.4 0.12 –0.47 2961.2/3018.4 1.6 –3.3 1.1 Fe 2395.6 0.01 2395.6/3018.4 0.014–0.094% 3.9 Mg 2852.1 0.002 2790.8/3018.4 0.023 –0.076 0.034% 2.3 Mn 2949.2/3058.8 0.87 b. C =60 μ f, L =480 μ h, R =50 ohms. Al 3059.9/2542.3 3.5 –4.5% 2.2% Cu 2961.2/2542.3 0.2 –1.3 1.3 2882.9/2542.3 1.0 –3.5 1.56% Pb 2833.1 0.0006% 2833.1/2670.5 0.002 –0.025 0.195 1.1 Fe 3020.6 0.0007 2994.4/2542.3 0.014–0.07% 0.0285 2.3 Mg 2852.1 0.0002 2783.0/2542.3 0.025 –0.07 0.0485 1.1 Cd 2288.0 0.0002 2288.0/2542.3 0.0015–0.003 2.0 Sn 3175.1 0.0005 3175.1/2542.3 0.00102 2.0
* Percent at which the intensity ratio of the line pair given is equal to one.
Table VIII
Data for the analysis of aluminum bronze. C =5 μ f, L =100 μ h, R =10 ohms.
Range Sensitivity (I =0.3 background) Line pair Working curve linear at 45° Working curve self-absorbed Index point* Precision (% average deviation) Cu 2882.9/2441.6 75.0 –95.0%** 1.8% Al 2660.4/2882.9 7.4 –17.0 0.50 Fe 2832.4/2882.9 1.0 –5.5 3.45% 1.0 Ni 3414.8 0.02% 3037.9/2882.9 0.1 –4.0% 0.77 0.83 Zn 3345.0 0.02 3302.6/2882.9 0.17 –2.4 0.56 0.82 Pb 2833.1 0.04 2833.1/2882.9 0.055–1.3 0.95 1.9 Sn 3175.1 0.04 3034.1/2882.9 0.16 –1.3 1.08 1.4 Mn 4030.8 0.005 2933.1/2882.9 0.01 – 0.06 0.06 –0.46 0.061 0.63 Si 2881.6 0.001 2881.6/2882.9 0.051– 0.29 0.172 1.8 Transmission readings (%) Av. dev. of I Mn 2933.1 28.8 28.0 29.8 28.3 28.8 28.5 28.9 29.0 1.1% Cu 3010.8 34.8 34.4 35.8 34.3 34.4 34.1 34.3 34.3 0.94 Intensity ratios Av. dev.
I
2933.1
Mn
I
3010.8
Cu 1.19 1.21 1.19 1.19 1.18 1.19 1.18 1.17 0.01
* Percent at which the intensity ratio of the line pair given is equal to one.
** Linear but not at 45°. See
Fig. 6 .