測(cè)定元素 氧氮?dú)淙?nbsp;可以同時(shí)得到氧氮?dú)淙齻€(gè)元素的結(jié)果。也可以單獨(dú)作為氧氮分析,和定氫的分析。 2 分析方法 惰性氣體脈沖加熱熔融方式 O 非色散紅外吸收法檢測(cè) N TCD熱導(dǎo)法檢測(cè) H 非色散紅外吸收法檢測(cè) 紅外法測(cè)量氫的技術(shù)早在70年代力可的碳?xì)涞治鰞x器上就已經(jīng)成熟使用,氫的精度有保證。關(guān)于市場(chǎng)上其他廠商的誤導(dǎo)用戶說(shuō)法,力可愿意以現(xiàn)實(shí)的調(diào)研數(shù)據(jù)說(shuō)話。標(biāo)書后頁(yè)附上了TCH600在用戶處的實(shí)際調(diào)研數(shù)據(jù),以作證明。 對(duì)于氧的檢測(cè),力可公司采用目前世界上的分析技術(shù),同時(shí)檢測(cè)CO和CO2,然后在轉(zhuǎn)化為CO2集中檢測(cè),原理上是zui完善的,所以不僅可以保證中間量程的氧的測(cè)量精度,在超低含量和高含量的檢測(cè)范圍內(nèi)同樣可以滿足精度要求。 力可TCH600儀器精度達(dá)到0.025ppm,高于其他供貨商一個(gè)數(shù)量級(jí),是目前市場(chǎng)上zui高的精度。
Sampling and sample preparation of refractory metals such as titanium and zirconium is somewhat different from that of
steel. Unlike steel samples, hydrogen is not as in this group of materials; therefore, storage in liquid nitrogen or dry ice is not required. However, it is important to keep the sample cool when cutting or sectioning. Sample preparation for
oxygen and nitrogen determination has been different from that for hydrogen determination. Typically, titanium and zirconium samples are chemically etched to remove surface contamination when oxygen and nitrogen are determined. However, etching can introduce hydrogen into the sample. ASTM method
E 1409 "Determination of Oxygen and Nitrogen in Titanium and Titanium Alloys by the Inert Gas Fusion
Technique", as updated in 1996, permits either etching or abrading (filing) of the test specimen. ASTM
E 1937 "Determination of Nitrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Technique" indicates that the test specimen be etched. ASTM E 1447 "Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity/Infrared Detection Method" permits surface preparation by abrading (if necessary to remove contamination). Differences in sample preparation
present somewhat of a dilemma regarding simultaneous determination of O, N, and H in Titanium. However, abrading samples with a file to remove surface contamination will yield accurate O, N, and H results.
O,NandHcontent.Thesebasketscan be used directly from the bottle without additional cleaning. To avoid contamination handle with clean forceps only.
CalibrationSamples
Refractory metal reference materials (titanium, zirconium, etc.) from LECO, NIST or other suitable reference materials.
SampleWeight
0.1 to 0.15 g
*RefractoryMetals include Ti, Zr, W, Mo, Ta, Nb, Hf, and their alloys.
TCH600
MethodParameters
AnalysisParameters
Outgas Cycles 3
Analysis Delay 20 seconds
Analysis Delay Comparator 1.000
Analysis Type Semi-Auto Analysis¹
¹Inearliersoftware programs this is the same as Auto Analysis. Auto Analysis is now used for instruments equipped with auto-sample loading capability, refer to the latest version of the operator's instruction manual for additional details.
ElementParameters Oxygen Nitrogen Hydrogen
Minimum Analysis Time
40 seconds
60 seconds
60 seconds
Significant Digits
5
5
6
Conversion Factor
1.00000
1.00000
1.00000
Integration Delay
5 seconds
15 seconds
10 seconds
Comparator Level
1.00000
1.00000
5.00000
Stop if below (%)
0.000000
0.000000
0.000000
FurnaceParameters
Furnace Control Mode Power
Pre-Analyze Purge Time —
Purge Time 10 seconds Outgas Time 15 seconds Outgas Cool Time 5 seconds Outgas Low Power 6000 watts* Outgas High Power 6000 watts* Outgas Ramp Rate —
Analyze Low Power 5200 watts* Analyze High Power 5200 watts* Analyze Ramp Rate —
Sample Prep Time — Sample Prep Power — Temperature Sustain None
*Mayvary,dependingonlinevoltage.Levelcan be adjusted to facilitate recovery and/or reduce crucible burn-through.
Procedure—SolidSamples
1. Prepare instrument for operation as outlined in the operator's instruction manual.
2. Determine Blank.
a. Enter 1.0000 g weight into weight stack.
b. Press Loader Switch on front of furnace, after a short delay the loading head slide block will open.
c. Place a 502-344 Nickel Basket into open port at top of loading head.
d. Press Loader Switch again, the loading head slide block will close and the lower electrode will open.
e. Add ~75 to 100 mg of 501-073 Graphite Powder to a 776-247 Graphite Crucible.
f. Place crucible on electrode pedestal.
g. Press Loader Switch, the lower electrode will close and the analysis sequence will start and end automatically.
h. Repeat steps 2a through 2g a minimum of five times.
i. Set the blank following the procedure outlined in the operator's instruction manual.
3. Calibrate/Drift Correct.
a. Weigh ~0.1 to 0.15 g of a calibration sample and enter weight into weight stack.
b. Place sample into a 502-344 Nickel Basket.
c. Press Loader Switch on front of furnace, the loading head slide block will open.
d. Place nickel basket/sample into open port at top of loading head.
e. Press Loader switch again, the loading head slide block will close and the lower electrode will open.
f. Add ~75 to 100 mg of 501-073 Graphite Powder to a 776-247 Graphite Crucible.
g. Place crucible on the electrode pedestal.
h. Press Loader Switch, the lower electrode will close and the analysis sequence will start and end automatically.
i. Repeat steps 3a through 3h a minimum of five times for each calibration sample used.
j. Calibrate or Drift Correct the instrument following the procedure outlined in the operator's instruction manual.
4. Analyze Samples
a. Weigh ~0.1 to 0.15 g sample and enter weight into weight stack. b. Proceed as directed in steps 3b through 3h.
TypicalResults—SolidSamples
Sample
Weightg
O%
N%
Hppm
LECO
0.1143
0.269
0.0174
11
502-201
0.1138
0.267
0.0161
11
Titanium Pin
0.1139
0.266
0.0174
11
0.267% O
0.1142
0.266
0.0172
13
0.017%N
0.1146
0.269
0.0167
12
0.1126
0.269
0.0173
12
0.1149
0.265
0.0170
12
0.1145
0.266
0.0172
12
0.1140
0.267
0.0164
12
0.1144
0.266
0.0171
12
X=
0.267
0.0170
12
s=
0.0016
0.0004
0.5
LECO
0.1086
0.131
0.0028
19
502-047
0.1111
0.131
0.0028
20
Zirconium Pin
0.1103
0.131
0.0029
20
0.13% O
0.1141
0.131
0.0028
20
0.1110
0.130
0.0025
19
0.1096
0.131
0.0029
20
0.1125
0.131
0.0029
20
0.1052
0.131
0.0027
19
0.1003
0.131
0.0027
20
0.1132
0.132
0.0029
20
X=
0.131
0.0028
20
s=
0.0004
0.0001
0.5
Procedure—Powder/ChipSamples
1. Prepare instrument for operation as outlined in the operator's instruction manual.
2. Determine Blank.
a. Enter 1.0000 g weight into weight stack.
b. Press Loader Switch on front of furnace, after a short delay the loading head slide block will open.
c. Insert a 501-059 Tin Capsule (leave capsule open) into a 502-344 Nickel Basket and place into open port at top of loading head.
d. Press Loader Switch again, the loading head slide block will close and the furnace lower electrode will open.
e. Add ~75 to 100 mg of 501-073 Graphite Powder to a 776-247 Graphite Crucible.
f. Place crucible on the furnace electrode pedestal.
g. Press Loader Switch, the lower electrode will close and the analysis sequence will start and end automatically.
h. Repeat steps 2a through 2g a minimum of five times.
i. Set blank following the procedure outlined in the operator's instruction manual.
3. Calibrate/Drift Correct.
a. Weigh ~0.1 to 0.15 g refractory metal calibration sample into a 501-059 Tin Capsule and enter weight into weight stack. Note: Calibration samples can be solid; they do not have to be powder
orchip.
b. Press Loader Switch on front of furnace, after a short delay the loading head slide block will open.
c. Insert capsule into 502-344 Nickel Basket and place into open port at top of loading head.
d. Press Loader Switch again, the loading head slide block will close and the furnace lower electrode will open.
e. Add ~75 to 100 mg of 501-073 Graphite Powder to a 776-247 Graphite Crucible.
f. Place crucible on furnace electrode pedestal.
g. Press Loader Switch, the lower electrode will close and the analysis sequence will start and end automatically.
h. Repeat steps 3a through 3g a minimum of five times for each calibration sample used.
i. Calibrate or Drift Correct the instrument following the procedure outlined in the operator's instruction manual.
4. Analyze Samples.
a. Weigh ~0.1 to 0.15 g sample into a 501-059 Tin Capsule and enter weight into weight stack.