3 分析范圍 氧0.05ppm-5%
氮0.05ppm-3%
氫 0.1ppm-0.25%
4 標準樣品重量 標準1.0g
5 分析精度（重現(xiàn)性）：
（氣標） O: 0.025ppm或0.5%RSD
N: 0.025ppm或0.5%RSD
H: 0.05ppm或2%RSD 氧氮的儀器分析精度，只有力可可以達到0.025ppm.
而其他廠商最高的精度只有0.2ppm,比力可低一個數(shù)量級。
6 靈敏度(最小讀數(shù)) O/N/H : 0.001ppm
7 分析時間 標準調(diào)置90秒（可根據(jù)具體分析選擇時間） 由于不再需要用色譜柱分離N2和H2，分析時間由原來180秒縮短到90秒，適合現(xiàn)場大分析量的應用。目前只有力可公司的TCH600可以滿足這個分析時間的要求。
其他廠商單測氫的時間為180秒，而得出氧氮氫三個結(jié)果的時間至少30分鐘，才可以保證精度。
8 脈沖電極加熱爐 1.高精度電流、電壓、功率控制功能，可以進行程序升溫分析，而且可以進行無極升溫。
2.爐子輸出功率：7.5KW，能滿足有色金屬、黑色金屬及各類高溫合金的檢測要求
3．電極爐自動定溫保持功能
4．系統(tǒng)漏氣檢查自動化，可進行爐頭漏氣分段控制進行檢漏
5.五步脫氣功能：在分析時可以提前將坩鍋中的雜氣經(jīng)5步脫氣用于降低空白 1．力可升溫程序可以任意設置，而其他廠商最多只能設定10段升溫。
2．力可儀器氣路漏氣檢查分為更詳細的4段檢漏，大大縮短了排查時間，其他廠商最多2路檢漏。
9 水循環(huán)方式 氧氮氫分析的釋放溫度很高，大約在3000攝氏度左右，單一的內(nèi)循環(huán)無法保證完全的冷卻，對儀器下電極的保護不夠。因此力可采用內(nèi)外冷卻循環(huán)水結(jié)合，確保冷卻效果。
六 分析軟件
1 操作界面 中文、英文操作界面 力可為出廠標準配置的多語言操作平臺（內(nèi)置包括英文和中文在內(nèi)的5種語言），而其他廠商為國內(nèi)翻譯，有軟件的沖突，容易死機。
2 報表功能 標準配置（儀器軟件自帶）
3 分析通道 氧氮氫通道無限制，用戶可自行編輯較為靈活的分析方法 其他廠商為最多16個通道。
4 分析功能 1. 分析模式：手動和自動分析
2. 分析條件：可設定溫度進行升溫分析�？梢匀我庠O定積分時間及累計積分
3. 校正：一點或多點校正，可對校正系數(shù)及校正曲線進行打印刪除校正數(shù)據(jù)功能。
分析結(jié)果可轉(zhuǎn)用于校正功能。
校正式補償功能
4. 分析結(jié)果可自動存儲、適時顯示、實時打印
5. 可實時動態(tài)顯示試樣的燃燒釋放曲線
6. 自動存儲分析圖形
7. 可顯示分析氣路
8. 在分析氣路可實現(xiàn)檢漏及機械、信號、輸出等自診斷功能
9. 遇異常情況可及時報警
10. 具備氧化物及氮化物分離的專用軟件
5 數(shù)據(jù)處理功能 平均值、標準偏差、相對標準偏差等
可對數(shù)據(jù)進行非連續(xù)性選擇
分析數(shù)據(jù)可及時進行網(wǎng)絡傳輸
分析結(jié)果可隨時轉(zhuǎn)化成分析報告
6 日志文件功能 記錄所有的操作、結(jié)果、維護，以便了解儀器運行狀況
7 幫助文件功能 1． 含維護、參考、操作手冊，提供具體的操作方法、故障產(chǎn)生的原因及排除方法，以便隨時查閱
2． 軟件配有HELP文件，可隨時查看
8 自診斷功能 警告性警報
提示性警報
七 技術服務
1 技術資料 賣方在合同生效后一個月內(nèi)寄發(fā)安裝條件說明書（中文）
由賣方負責安裝、調(diào)試。正常運轉(zhuǎn)驗收合格后方能交付使用。
賣方提供中英文操作手冊、維修手冊、電路圖等技術手冊一式兩份。
2 儀器驗收 按標樣分析精度要求和中短期精度試驗指標進行考核。
3 售后服務 廠家在國內(nèi)要有維修中心，要有專職的維修工程師，設有備品備件庫，在買方提出維修要求后，能在4小時內(nèi)做出維修響應，1－2個工作日內(nèi)到達用戶現(xiàn)場：供方應負責終身維修。 目前只有力可在國內(nèi)設有維修中心，力可為廠商直銷，在上海設有總代表處，在北京和重慶設有分支機構(gòu)，為中國用戶服務超過了30年。力可的維修工程師均為專職，在國內(nèi)共有11名。
其他廠商為代理制銷售，售后服務實力無法保障。
4 培訓 免費提供2-4人國內(nèi)一周培訓。包括儀器基本原理、使用維護要求常見故障現(xiàn)象及排除的培訓。在儀器安裝調(diào)試時，賣方安裝工程師對用戶現(xiàn)場進行技術培訓，著重儀器硬件的檢修培訓。
5 質(zhì)量保證期 儀器整機保修12個月，保修期內(nèi)接到維修邀請應在電話中即刻答復或8小時內(nèi)派員到場修復。
Oxygen, Nitrogen, and Hydrogen Determination
in Refractory Metals*
Instrument
TCH600
Sampling and Sample Preparation
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 mobile 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.
Accessories
776-247 Graphite Crucibles, 501-073 Graphite Powder, 502-344 Nickel Basket, 501-059 Tin Capsule
(powder, chip, granular samples)
Note: LECO 502-344 Nickel Baskets are prepared using a proprietary procedure to ensure low and precise
O, N and H content. These baskets can be used directly from the bottle without additional cleaning. To avoid contamination handle with clean forceps only.
Calibration Samples
Refractory metal reference materials (titanium, zirconium, etc.) from LECO, NIST or other suitable reference materials.
Sample Weight
0.1 to 0.15 g
*Refractory Metals include Ti, Zr, W, Mo, Ta, Nb, Hf, and their alloys.
TCH600
Method Parameters
Analysis Parameters
Outgas Cycles 3
Analysis Delay 20 seconds
Analysis Delay Comparator 1.000
Analysis Type Semi-Auto Analysis1
1In earlier software 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.
Element Parameters 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 |
Furnace Parameters
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
*May vary, depending on line voltage. Level can be adjusted to facilitate recovery and/or reduce crucible burn-through.
Procedure—Solid Samples
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.
Typical Results—Solid Samples
|
Sample |
Weight g |
O % |
N % |
H ppm |
|
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/Chip Samples
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
or chip.
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.
b. Proceed as directed in 3b through 3g.
Typical Results—Powder Samples
|
Sample |
Weight g |
O % |
N % |
H ppm |
|
Tantalum |
0.1055 |
0.206 |
0.0045 |
38 |
|
Powder |
0.1076 |
0.207 |
0.0045 |
39 |
|
|
0.1096 |
0.205 |
0.0040 |
37 |
|
|
0.1020 |
0.205 |
0.0044 |
38 |
|
|
0.1052 |
0.206 |
0.0048 |
39 |
|
|
X = |
0.206 |
0.0045 |
38 |
|
|
s = |
0.001 |
0.0003 |
1 |
